CN1724165A - Process of treating catalyst carrier waste active carbon for synthesizing vinyl acetate - Google Patents
Process of treating catalyst carrier waste active carbon for synthesizing vinyl acetate Download PDFInfo
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- CN1724165A CN1724165A CNA2005100108411A CN200510010841A CN1724165A CN 1724165 A CN1724165 A CN 1724165A CN A2005100108411 A CNA2005100108411 A CN A2005100108411A CN 200510010841 A CN200510010841 A CN 200510010841A CN 1724165 A CN1724165 A CN 1724165A
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- active carbon
- vinyl acetate
- catalyst carrier
- waste active
- heating
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 title claims description 59
- 239000002699 waste material Substances 0.000 title claims description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 3
- 230000003213 activating effect Effects 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 18
- 230000004913 activation Effects 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000003672 processing method Methods 0.000 claims description 10
- 239000001569 carbon dioxide Substances 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000005554 pickling Methods 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract 2
- 230000001172 regenerating effect Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 15
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000011084 recovery Methods 0.000 description 8
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 7
- 229910052740 iodine Inorganic materials 0.000 description 7
- 239000011630 iodine Substances 0.000 description 7
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 7
- 229960000907 methylthioninium chloride Drugs 0.000 description 7
- 239000002156 adsorbate Substances 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000013904 zinc acetate Nutrition 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- OOVXWEQVEHIHSO-UHFFFAOYSA-N acetic acid ethene Chemical compound C=C.C=C.C=C.CC(O)=O OOVXWEQVEHIHSO-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
A process for regenerating the used activated carbon as the carrier of catalyst for synthesizing vinyl acetate includes such steps as drying, putting it in reacting ceramic or quart2 tube, microwave heating, activating by introducing CO2 or steam, washing with sulfuric acid, rinsing with distilled water until it become neutral, and baking.
Description
The catalyst carrier waste active carbon for synthesizing vinyl acetate processing method the invention belongs to waste recovery and comprehensive utilization technique field.
Vinyl acetate is a kind of important synthetic material monomer, is mainly used in the adhesive of industries such as manufacturing emulsion paint and building, weaving, packing, is unique initiation material of broad-spectrum polyvinyl alcohol and acetals series of products thereof.Vinyl acetate is to be raw material with acetylene and acetate in the industrial production, and it is synthetic to carry out gas phase catalysis under the effect of catalyst, and its catalyst is a zinc acetate, and catalyst carrier is an active carbon.Because acetylene and acetate gas phase catalysis synthesis of acetic acid ethene are quick exothermic reactions, in the catalyst use,, cause active carbon pore structure to be damaged because of local high heat produces sintering; In addition, catalyst surface carbonyl content a large amount of minimizing in reaction process makes the decline of catalyst surface chemism, can lose activity after causing catalyst to use a period of time in process of production, causes a large amount of discarded of catalyst carrier.There are tens families in the producer that uses the carbon compositing catalyst carrier to carry out large-scale production in China, needs kiloton on the discarded active carbon every year.If a large amount of discarded catalyst carrier active carbons are not recycled, will cause the significant wastage of resource.And,,, will cause environmental pollution if it is not handled owing to adsorbed a large amount of zinc acetates in the activated carbon capillary that goes out of use.So, the vinyl acetate synthetic catalyst carrier waste active carbon of being discarded in the vinyl acetate production is handled and utilized, aspect comprehensive utilization of resources, have profound significance.
At present, processing method to waste active carbon can be divided into two classes: the one, manage to make the adsorbate desorption, promptly introduce material or energy and make reaction force attenuation or disappearance between adsorption molecule and the active carbon, finally remove adsorbate, reach the purpose that active carbon recovers its absorption property; The 2nd, make adsorbent generation thermal decomposition or redox reaction, reach and remove the purpose that adsorbate recovers the charcoal absorption performance.Though known waste active carbon processing method technology is ripe, also has a lot of shortcomings in processing procedure: need a large amount of energy heating in (1) processing procedure, investment and operating cost are higher; (2) processing time is long; (3) handle the back active carbon and burn mistake seriously, the rate of recovery is low; (4) charcoal absorption performance after treatment can reduce.
The object of the present invention is to provide a kind of processing method of catalyst carrier waste active carbon for synthesizing vinyl acetate.The charcoal absorption performance that method obtains is good, rate of recovery height, and technology is simple and easy to do.
Technical characterictic of the present invention is to be placed on the catalyst carrier waste active carbon for synthesizing vinyl acetate drying in the quartzy or ceramic reaction tube of heating using microwave and to heat in microwave field, use chlorohydric acid pickling after feeding carbon dioxide or steam activation then, carry out repeatedly rinsing with distilled water again, dry to neutral back and obtain active carbon finished products.
Its concrete processing step is as follows, and its process flow diagram shows at Figure of description: (1) places baking oven with catalyst carrier waste active carbon for synthesizing vinyl acetate, and is following dry 2～5 hours 100 ℃～120 ℃ of temperature; (2) dried waste active carbon is placed the quartzy or ceramic reaction tube of heating using microwave and put into microwave heating equipment and heated 2～5 minutes; Make adsorbate decompose and desorption microwave power 0.1～80KW, frequency 2450MH, (3) in quartzy or ceramic reaction tube, fed carbon dioxide or steam 5～30 minutes, make the active carbon activation, 0.1～30 liter/minute of activated gas flow, 600 ℃～900 ℃ of activation temperatures;
(4) the active carbon weight percent concentration that activation is obtained is 3% salt acid elution 1～5 time, reaches 4.0～7.0 with distilled water rinsing to pH value then; (5) active carbon after the rinsing places baking oven drying under 100 ℃～120 ℃ temperature to obtain active carbon finished products in 2～5 hours.
The present invention has the following advantages: advantages such as (1) utilizes microwave homogeneous heating to be arranged directly to the heating of material inside, and speed is fast, make the waste active carbon processing procedure time few (processing procedure only needs 30 minutes), treatment temperature is low, consuming little energy, and the active carbon loss on ignition is few, rate of recovery height; (2) use good and can resistant to elevated temperatures quartz or ceramic reaction tube to the microwave wave penetrate capability, microwave energy utilization rate height; (3) active carbon is inner to produce a large amount of active sites because heating using microwave can make, and feeds carbon dioxide or steam makes active carbon activate pore-creating once more in processing procedure, has overcome the shortcoming that the charcoal absorption performance reduces behind the known process waste active carbon; (4) introduce carbon dioxide or steam active carbon is activated once more, the activated carbon product absorption property after the processing is good, the primes active carbon requirement that its iodine sorption value, methylene blue adsorption value can be up to state standards and require.(5) technological operation is simple, is easy to control.
Embodiment
Embodiment 1
With Yunnan one chemical plant catalyst carrier waste active carbon for synthesizing vinyl acetate is raw material, and its iodine sorption value is 361mg/g after dezincify is handled, and methylene blue adsorption value is 45mg/g.Waste active carbon was put into crystal reaction tube after under 120 ℃ the temperature dry 3 hours, in frequency is 2450MHz, power is heating 3 minutes in the micro-wave oven of 1.2KW, the carbon dioxide activation that feeds flow then and be 0.8L/min obtained active carbon after 20 minutes, the active carbon weight percent concentration be behind 3% the chlorohydric acid pickling 2 times with the distilled water rinsing to pH value to 6.0, under 120 ℃ temperature, obtained the finished product active carbon in dry 4 hours.
Its experimental condition and testing result such as table one:
Table one: heating using microwave carbon dioxide activation processing waste active carbon experimental condition and index
| Experimental condition | Testing result | |||||
| Microwave power (KW) | Activation temperature (min) | Soak time (min) | Carbon dioxide flow (L/min) | Iodine sorption value (mg/g) | Methylene blue adsorption value (mg/g) | The rate of recovery (%) |
| 1.2 | 800℃ | 20 | 0.8 | 1158.02 | 240 | 86.45 |
As can be seen from the above table, the waste active carbon absorption property that adopts the present invention to handle is good, its iodine sorption value, methylene blue adsorption value are respectively 1158.02mg/g and 240mg/g, the primes active carbon requirement that is up to state standards and requires. and the rate of recovery is up to 86.45%.
Embodiment 2
With Yunnan one chemical plant catalyst carrier waste active carbon for synthesizing vinyl acetate is raw material, and its iodine sorption value is 361mg/g after dezincify is handled, and methylene blue adsorption value is 45mg/g.Waste active carbon was put into crystal reaction tube after under 100 ℃ the temperature dry 4 hours, in frequency is 2450MHz, power is heating 2 minutes in the microwave field of 1.5KW, the steam activation that feeds flow then and be 0.5L/min obtained active carbon after 15 minutes, the active carbon weight percent concentration be behind 3% the chlorohydric acid pickling 2 times with the distilled water rinsing to pH value to 6.0, under 100 ℃ temperature, obtained the finished product active carbon in dry 5 hours.
Its experimental condition and testing result such as table two:
Table two: the heating using microwave steam activation is handled waste active carbon experimental condition and index
| Experimental condition | Testing result | |||||
| Microwave power (KW) | Activation temperature (min) | Soak time (min) | Steam flow (L/min) | Iodine sorption value (mg/g) | Methylene blue adsorption value (mg/g) | The rate of recovery (%) |
| 1.5 | 700℃ | 15 | 0.5 | 1193.85 | 285 | 76.36 |
As can be seen from the above table, the waste active carbon absorption property that adopts the present invention to handle is good, its iodine sorption value, methylene blue adsorption value are respectively 1193.85mg/g and 285mg/g, the primes active carbon requirement that is up to state standards and requires, and the rate of recovery can reach 76.36%.
Claims (6)
1. catalyst carrier waste active carbon for synthesizing vinyl acetate processing method, it is characterized in that being placed on the catalyst carrier waste active carbon for synthesizing vinyl acetate drying in the quartzy or ceramic reaction tube of heating using microwave and in microwave field, heating certain hour, feed then behind carbon dioxide or the steam activation certain hour with chlorohydric acid pickling and carry out repeatedly rinsing, obtain active carbon finished products to the oven dry under 100 ℃～120 ℃ temperature of neutral back with distilled water again.
2. as claim 1 described catalyst carrier waste active carbon for synthesizing vinyl acetate processing method, it is characterized in that waste active carbon was in the past will be under 100 ℃～120 ℃ temperature with microwave treatment dry 2～5 hours.
3. as claim 1 described catalyst carrier waste active carbon for synthesizing vinyl acetate processing method, its processing procedure is to carry out in heating using microwave quartz or ceramic reaction tube, microwave heating equipment power 0.1～80KW, frequency 2450MHz, waste active carbon need heating 2～5 minutes in microwave field.
4. as claim 1 or 3 described catalyst carrier waste active carbon for synthesizing vinyl acetate processing methods, it is characterized in that heating back feeding carbon dioxide or steam activates waste active carbon, the activated gas flow is 0.1～30 liter/minute, 600～900 ℃ of activation temperatures, soak time are 5～30 minutes.
5. as claim 1 described catalyst carrier waste active carbon for synthesizing vinyl acetate processing method, it is characterized in that activating the active carbon that obtains need be 3% chlorohydric acid pickling 1～5 time with concentration, reaches 4.0～7.0 with distilled water rinsing to pH value then.
6. as claim 1 or 5 described microwave heating treatment catalyst carrier waste active carbon for synthesizing vinyl acetate methods, it is characterized in that the active carbon after washing need drying obtain active carbon finished products in 2～5 hours under 100 ℃～120 ℃ temperature.
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| CNB2005100108411A CN100482348C (en) | 2005-06-07 | 2005-06-07 | Process of treating catalyst carrier waste active carbon for synthesizing vinyl acetate |
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| CNB2005100108411A CN100482348C (en) | 2005-06-07 | 2005-06-07 | Process of treating catalyst carrier waste active carbon for synthesizing vinyl acetate |
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| CN1724165A true CN1724165A (en) | 2006-01-25 |
| CN100482348C CN100482348C (en) | 2009-04-29 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103071455A (en) * | 2013-02-26 | 2013-05-01 | 昆明理工大学 | Preparation method of composite adsorption purifying agent |
| CN103691396A (en) * | 2014-01-22 | 2014-04-02 | 湖北君集水处理有限公司 | System and method for powdered activated carbon regeneration through microwaves |
| CN105293489A (en) * | 2015-11-16 | 2016-02-03 | 昆明理工大学 | Regeneration method of waste active carbon for monosodium glutamate by supersonic wave and spray |
| CN105905897A (en) * | 2015-07-01 | 2016-08-31 | 洛阳名力科技开发有限公司 | Preparation method of active carbon for waste water treatment |
| CN107670455A (en) * | 2017-11-02 | 2018-02-09 | 苏州太平洋印务有限公司 | Printing industry exhaust-gas treatment and regeneration method of active carbon |
| CN111068792A (en) * | 2018-10-18 | 2020-04-28 | 中国石油化工股份有限公司 | Regeneration method of waste catalyst for synthesizing vinyl acetate by acetylene method |
| CN112871132A (en) * | 2019-11-29 | 2021-06-01 | 中国石油天然气集团有限公司 | Carbonyl activated carbon particles and preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334237C (en) * | 2003-08-30 | 2007-08-29 | 大连理工大学 | Reproducing method for carrier gold activated carbon |
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2005
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103071455A (en) * | 2013-02-26 | 2013-05-01 | 昆明理工大学 | Preparation method of composite adsorption purifying agent |
| CN103691396A (en) * | 2014-01-22 | 2014-04-02 | 湖北君集水处理有限公司 | System and method for powdered activated carbon regeneration through microwaves |
| CN105905897A (en) * | 2015-07-01 | 2016-08-31 | 洛阳名力科技开发有限公司 | Preparation method of active carbon for waste water treatment |
| CN105293489A (en) * | 2015-11-16 | 2016-02-03 | 昆明理工大学 | Regeneration method of waste active carbon for monosodium glutamate by supersonic wave and spray |
| CN105293489B (en) * | 2015-11-16 | 2018-03-06 | 昆明理工大学 | A kind of method of ultrasonic atomization regenerating waste monosodium glutamate activated carbon |
| CN107670455A (en) * | 2017-11-02 | 2018-02-09 | 苏州太平洋印务有限公司 | Printing industry exhaust-gas treatment and regeneration method of active carbon |
| CN107670455B (en) * | 2017-11-02 | 2020-09-15 | 苏州太平洋印务有限公司 | Waste gas treatment and active carbon regeneration method in printing industry |
| CN111068792A (en) * | 2018-10-18 | 2020-04-28 | 中国石油化工股份有限公司 | Regeneration method of waste catalyst for synthesizing vinyl acetate by acetylene method |
| CN112871132A (en) * | 2019-11-29 | 2021-06-01 | 中国石油天然气集团有限公司 | Carbonyl activated carbon particles and preparation method and application thereof |
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| Publication number | Publication date |
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| CN100482348C (en) | 2009-04-29 |
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