CN107175091A - A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way - Google Patents

A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way Download PDF

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Publication number
CN107175091A
CN107175091A CN201710434913.8A CN201710434913A CN107175091A CN 107175091 A CN107175091 A CN 107175091A CN 201710434913 A CN201710434913 A CN 201710434913A CN 107175091 A CN107175091 A CN 107175091A
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carbon molecular
nitrogen
activating
molecular sieve
molecular sieves
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陈丽莎
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Huzhou Informed Technology Service Co Ltd
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Huzhou Informed Technology Service Co Ltd
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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
    • B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
    • 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
    • B01J20/3458—Regenerating or reactivating using a particular desorbing compound or mixture in the gas phase
    • 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
    • B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Treating Waste Gases (AREA)

Abstract

The invention discloses a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that comprises the following steps：（1）Screening, cleaning；（2）Carbonization；（3）Mixed gas is activated；（4）Carbon deposition；（5）Finished product.A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way of the present invention, realizes the carbon molecular sieve for " being poisoned " deeper by the production technology of activating and regenerating and recycles, obtain the preferable carbon molecular sieve of quality, realize the recycling of Industrial Solid Waste.

Description

A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way
Technical field
The present invention relates to a kind of carbon molecular sieve activating and regenerating Application way, particularly a kind of poison deactivation nitrogen-preparing carbon molecular sieves Activating and regenerating Application way.
Background technology
Nitrogen-preparing carbon molecular sieves are used to separate air enrichment nitrogen, using Room-temperature low-pressure nitrogen producing craft, higher than traditional deep cooling Pressure nitrogen producing craft has investment cost few, and production nitrogen speed is fast, nitrogen low cost and other advantages.Therefore, it is that current engineering circles are preferred Pressure-variable adsorption (abbreviation P.S.A) air separation nitrogen-enriching adsorbent, this nitrogen is in chemical industry, industrial gas oil, electronics work Extensive use in terms of industry, food industry, coal industry, medical industry, cable industry, metal heat treatmet, transport and storage.
The content of the invention
It is an object of the present invention to provide a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, passes through work Changing the production technology of regeneration makes the carbon molecular sieve for " being poisoned " deeper realize recycling, obtains the preferable carbon molecular sieve of quality, real The recycling of existing Industrial Solid Waste.
Technical scheme：A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that Comprise the following steps：
（1）Screening, cleaning：By mesh screen screening of the carbon molecular sieve of being poisoned through 15-30 mesh, then obtained carbon molecular sieve water will be screened Rinse 2-3 times, go the removal of impurity；
（2）Carbonization：The carbon molecular sieve cleaned is placed in flue, 700-1000 DEG C is warming up to and is carbonized；
（3）Mixed gas is activated：After high temperature cabonization, CO2, CO mixed gas are passed through into flue, the carbon molecular sieve of charing is entered Row activation, in-furnace temperature is 750-850 DEG C；
（4）Carbon deposition：Carbon molecular sieve after will be activated is placed in converter flue, and converter temperature is 800-900 DEG C, is protected in nitrogen Hole-blocking agent is passed through under shield, keeps furnace temperature to adsorb hole-blocking agent at 300-500 DEG C, then makes absorption in carbon materials at 800-900 DEG C Hole-blocking agent cracking on material, so that, aperture adjustment is carried out to carbon molecular sieve by pyrocarbon on the carbon material；
（5）Finished product：It is made after activating and regenerating nitrogen-preparing carbon molecular sieves, carries out screening packaging.
A kind of foregoing poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, the step（2）In, carbonization be Carried out under inert environments.
A kind of foregoing poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, the inert environments refer in nitrogen In the environment of.
A kind of foregoing poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, the step（3）In, CO2 ratios For 85%-90%, CO ratios are 10%-15%.
A kind of foregoing poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, the step（3）In, in-furnace temperature For 750 DEG C.
A kind of foregoing poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, the step（4）In, hole-blocking agent is Benzene, toluene or dimethylbenzene.
A kind of foregoing poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, the step（4）In, it is heavy by carbon Carbon molecular sieve micropore size after product can reach 0.28-0.3nm.
Compared with prior art, the present invention carries out aperture adjustment using Carbon deposition method to the carbon molecular sieve after activation, leads to Cross addition hole-blocking agent（Benzene or toluene or dimethylbenzene）, under the conditions of Pintsch process, make pyrocarbon in the porch of macropore, from And macropore diameter is reduced, product aperture is uniformed, the purpose of activating and regenerating is reached.
Due to the H adsorbed in the carbon molecular sieve micropore during nitrogen processed2O molecules and the greasy dirt on covering carbon molecular sieve surface with And other chemical contaminations, cause nitrogen-preparing carbon molecular sieves " poisoning ", and the reason for " poisoning " and degree is general all relatively deep, simply Complete activating and regenerating can not be accomplished during activation process.This kind of situation need to pass through high temperature carbonization, gas after early stage cleaning processing After activation process, it just can ensure that residuing in the higher boiling composition in adsorbed state in carbon molecular sieve micropore is heated and decomposes, A part of low molecule gasifies and desorbed, and remaining part turns into carbon.
After above-mentioned carbonization, activation process, make borehole enlargement scope needed for.But in actual production, by carbonization, live The carbon molecular sieve aperture of gained is also uneven after change, and macropore is more, and macropore diameter is typically in 0.5-0.55nm or so, and it separates empty Gas it is indifferent.Present invention introduces the method for Carbon deposition, by adding micropore regulator（Benzene or toluene or dimethylbenzene）, in height Under the conditions of anneal crack solution, make pyrocarbon in the porch of macropore, so as to reduce macropore diameter, uniform product aperture, reach It to the purpose of activating and regenerating, can recycle the nitrogen-preparing carbon molecular sieves that depth is poisoned.
Embodiment
The present invention is further illustrated for example below, but is not intended as to the foundation of the invention limited.
Embodiment 1：A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that including following Step：
（1）Screening, cleaning：Mesh screen screening of the carbon molecular sieve of being poisoned through 30 mesh, then the carbon molecular sieve that screening is obtained are rushed with water Wash 3 times, go the removal of impurity.
（2）Carbonization：The carbon molecular sieve cleaned is placed in flue, 700 DEG C are warming up under nitrogen protection and is carbonized, The impurity for making micropore internal congestion using the step is carbonized, and microporous molecular sieve is reopened, and reaches activating and regenerating effect.
（3）Mixed gas is activated：After high temperature cabonization, CO2, CO mixed gas, wherein CO are passed through into flue2Ratio is 85%, CO ratio are 15%, and the carbon molecular sieve of carbonization is activated, and in-furnace temperature is 750 DEG C.
（4）Carbon deposition：Carbon molecular sieve after will be activated is placed in converter flue, and converter temperature is 800 DEG C, is protected in nitrogen Dimethylbenzene is passed through under shield, keeps furnace temperature to adsorb dimethylbenzene at 500 DEG C.Then make at 800 DEG C absorption on the carbon material two Toluene is cracked, so that, aperture adjustment is carried out to carbon molecular sieve by pyrocarbon on the carbon material, the carbon after Carbon deposition point Son sieve micropore size can reach 0.28nm.
（5）Finished product：It is made after activating and regenerating nitrogen-preparing carbon molecular sieves, carries out screening packaging.
Embodiment 2：A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that including following Step：
（1）Screening, cleaning：Mesh screen screening of the carbon molecular sieve of being poisoned through 15 mesh, then the carbon molecular sieve that screening is obtained are rushed with water Wash 3 times, go the removal of impurity.
（2）Carbonization：The carbon molecular sieve cleaned is placed in flue, 1000 DEG C of progress charcoals are warming up under nitrogen protection Change, the impurity for making micropore internal congestion using the step is carbonized, and microporous molecular sieve is reopened, and reaches activating and regenerating effect.
（3）Mixed gas is activated：After high temperature cabonization, CO2, CO mixed gas, wherein CO are passed through into flue2Ratio is 90%, CO ratio are 10%, and the carbon molecular sieve of carbonization is activated, and in-furnace temperature is 850 DEG C.
（4）Carbon deposition：Carbon molecular sieve after will be activated is placed in converter flue, and converter temperature is 900 DEG C, is protected in nitrogen Toluene is passed through under shield, keeps furnace temperature to adsorb toluene at 500 DEG C.Then split at 900 DEG C the toluene of absorption on the carbon material Solution, so that, aperture adjustment is carried out to carbon molecular sieve, the carbon molecular sieve after Carbon deposition is micro- by pyrocarbon on the carbon material Hole aperture can reach 0.28-0.nm.
（5）Finished product：It is made after activating and regenerating nitrogen-preparing carbon molecular sieves, carries out screening packaging.
Embodiment 3：A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that including following Step：
（1）Screening, cleaning：Mesh screen screening of the carbon molecular sieve of being poisoned through 30 mesh, then the carbon molecular sieve that screening is obtained are rushed with water Wash 2 times, go the removal of impurity.
（2）Carbonization：The carbon molecular sieve cleaned is placed in flue, 700 DEG C are warming up under nitrogen protection and is carbonized, The impurity for making micropore internal congestion using the step is carbonized, and microporous molecular sieve is reopened, and reaches activating and regenerating effect.
（3）Mixed gas is activated：After high temperature cabonization, CO2, CO mixed gas, wherein CO are passed through into flue2Ratio is 90%, CO ratio are 10%, and the carbon molecular sieve of carbonization is activated, and in-furnace temperature is 850 DEG C.
（4）Carbon deposition：Carbon molecular sieve after will be activated is placed in converter flue, and converter temperature is 800 DEG C, is protected in nitrogen Benzene is passed through under shield, keeps furnace temperature to adsorb benzene at 300 DEG C.Then the benzene cracking of absorption on the carbon material is made at 900 DEG C, so that By pyrocarbon on the carbon material, aperture adjustment, the carbon molecular sieve micropore size after Carbon deposition are carried out to carbon molecular sieve It can reach 0.3nm.
（5）Finished product：It is made after activating and regenerating nitrogen-preparing carbon molecular sieves, carries out screening packaging.
Embodiment 4：A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that including following Step：
（1）Screening, cleaning：Mesh screen screening of the carbon molecular sieve of being poisoned through 25 mesh, then the carbon molecular sieve that screening is obtained are rushed with water Wash 3 times, go the removal of impurity.
（2）Carbonization：The carbon molecular sieve cleaned is placed in flue, 900 DEG C are warming up under nitrogen protection and is carbonized, The impurity for making micropore internal congestion using the step is carbonized, and microporous molecular sieve is reopened, and reaches activating and regenerating effect.
（3）Mixed gas is activated：After high temperature cabonization, CO2, CO mixed gas, wherein CO are passed through into flue2Ratio is 88%, CO ratio are 12%, and the carbon molecular sieve of carbonization is activated, and in-furnace temperature is 800 DEG C.
（4）Carbon deposition：Carbon molecular sieve after will be activated is placed in converter flue, and converter temperature is 850 DEG C, is protected in nitrogen Dimethylbenzene is passed through under shield, keeps furnace temperature to adsorb dimethylbenzene at 400 DEG C.Then make at 900 DEG C absorption on the carbon material two Toluene is cracked, so that, aperture adjustment is carried out to carbon molecular sieve by pyrocarbon on the carbon material, the carbon after Carbon deposition point Son sieve micropore size can reach 0.29nm.
（5）Finished product：It is made after activating and regenerating nitrogen-preparing carbon molecular sieves, carries out screening packaging.
Embodiment 5：A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that including following Step：
（1）Screening, cleaning：Mesh screen screening of the carbon molecular sieve of being poisoned through 20 mesh, then the carbon molecular sieve that screening is obtained are rushed with water Wash 3 times, go the removal of impurity.
（2）Carbonization：The carbon molecular sieve cleaned is placed in flue, 800 DEG C are warming up under nitrogen protection and is carbonized, The impurity for making micropore internal congestion using the step is carbonized, and microporous molecular sieve is reopened, and reaches activating and regenerating effect.
（3）Mixed gas is activated：After high temperature cabonization, CO2, CO mixed gas, wherein CO are passed through into flue2Ratio is 90%, CO ratio are 10%, and the carbon molecular sieve of carbonization is activated, and in-furnace temperature is 820 DEG C.
（4）Carbon deposition：Carbon molecular sieve after will be activated is placed in converter flue, and converter temperature is 860 DEG C, is protected in nitrogen Toluene is passed through under shield, keeps furnace temperature to adsorb toluene at 450 DEG C.Then split at 850 DEG C the toluene of absorption on the carbon material Solution, so that, aperture adjustment is carried out to carbon molecular sieve, the carbon molecular sieve after Carbon deposition is micro- by pyrocarbon on the carbon material Hole aperture can reach 0.3nm.
（5）Finished product：It is made after activating and regenerating nitrogen-preparing carbon molecular sieves, carries out screening packaging.

Claims (7)

1. a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way, it is characterised in that comprise the following steps：
（1）Screening, cleaning：By mesh screen screening of the carbon molecular sieve of being poisoned through 15-30 mesh, then obtained carbon molecular sieve water will be screened Rinse 2-3 times, go the removal of impurity；
（2）Carbonization：The carbon molecular sieve cleaned is placed in flue, 700-1000 DEG C is warming up to and is carbonized；
（3）Mixed gas is activated：After high temperature cabonization, CO is passed through into flue2, CO mixed gas, the carbon molecular sieve of charing is carried out Activation, in-furnace temperature is 750-850 DEG C；
（4）Carbon deposition：Carbon molecular sieve after will be activated is placed in converter flue, and converter temperature is 800-900 DEG C, is protected in nitrogen Hole-blocking agent is passed through under shield, keeps furnace temperature to adsorb hole-blocking agent at 300-500 DEG C, then makes absorption in carbon materials at 800-900 DEG C Hole-blocking agent cracking on material, so that, aperture adjustment is carried out to carbon molecular sieve by pyrocarbon on the carbon material；
（5）Finished product：It is made after activating and regenerating nitrogen-preparing carbon molecular sieves, carries out screening packaging.
2. a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way as claimed in claim 1, it is characterised in that institute State step（2）In, carbonization is to carry out in an inert atmosphere.
3. a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way as claimed in claim 2, it is characterised in that institute Inert environments are stated to refer in the environment of nitrogen.
4. a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way as claimed in claim 1, it is characterised in that institute State step（3）In, CO2Ratio is 85%-90%, and CO ratios are 10%-15%.
5. a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way as described in claim 1 or 4, its feature exists In the step（3）In, in-furnace temperature is 750 DEG C.
6. a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way as claimed in claim 1, it is characterised in that institute State step（4）In, hole-blocking agent is benzene, toluene or dimethylbenzene.
7. a kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way as claimed in claim 1, it is characterised in that institute State step（4）In, the carbon molecular sieve micropore size after Carbon deposition can reach 0.28-0.3nm.
CN201710434913.8A 2017-06-10 2017-06-10 A kind of poison deactivation nitrogen-preparing carbon molecular sieves activating and regenerating Application way Withdrawn CN107175091A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101708469A (en) * 2009-10-27 2010-05-19 湖州强马分子筛有限公司 Process for activating and regenerating nitrogen-preparing carbon molecular sieves
CN102784631A (en) * 2012-08-23 2012-11-21 长兴山立化工材料科技有限公司 Method for regenerating carbon molecular sieve
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
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101708469A (en) * 2009-10-27 2010-05-19 湖州强马分子筛有限公司 Process for activating and regenerating nitrogen-preparing carbon molecular sieves
CN102784631A (en) * 2012-08-23 2012-11-21 长兴山立化工材料科技有限公司 Method for regenerating carbon molecular sieve
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
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
应贤政 等: "碳分子筛活化再生技术的应用", 《大氮肥》 *

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Application publication date: 20170919