CN106433227B - A kind of processing of organic dead catalyst and reuse method - Google Patents
A kind of processing of organic dead catalyst and reuse method Download PDFInfo
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- CN106433227B CN106433227B CN201610792396.7A CN201610792396A CN106433227B CN 106433227 B CN106433227 B CN 106433227B CN 201610792396 A CN201610792396 A CN 201610792396A CN 106433227 B CN106433227 B CN 106433227B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000000889 atomisation Methods 0.000 claims abstract description 11
- 239000006229 carbon black Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000007885 magnetic separation Methods 0.000 claims abstract description 9
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 9
- 238000005507 spraying Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000004806 packaging method and process Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 36
- 150000007513 acids Chemical class 0.000 claims description 26
- 229910052755 nonmetal Inorganic materials 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 11
- 239000003250 coal slurry Substances 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000003518 caustics Substances 0.000 claims description 9
- 239000000446 fuel Substances 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 238000006053 organic reaction Methods 0.000 claims description 7
- 239000003034 coal gas Substances 0.000 claims description 5
- 239000003345 natural gas Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims 1
- 239000002910 solid waste Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 32
- 239000002893 slag Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000012216 screening Methods 0.000 description 6
- 238000003672 processing method Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
Processing and reuse method, step the invention discloses a kind of organic dead catalyst is as follows：(1) it is pressurizeed by nitrogen and organic dead catalyst is pressed into atomizer, spraying enters in rotary furnace, burns；Atomisation pressure is 0.1 0.5MPa, and incineration temperature is 500 900 DEG C, and the burning time is 60s；(2) it after step (1) products therefrom is cooled down, is delivered in reaction kettle, adds water, stir 30 40 minutes, filtering, filter residue is after liquid caustic soda neutralizes, then washing filtering is three times, obtains washings and filter residue；(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；(4) step (3) products therefrom be granulated, dried, being screened, magnetic separation, packaging, finished product carbon black.On the one hand the harmless treatment to organic dead catalyst is realized, dangerous solid waste is on the other hand changed into available product, while bringing benefits, solves the problems, such as environmental pollution.
Description
Technical field
Processing and reuse method the present invention relates to a kind of organic dead catalyst, and in particular to one kind is used for organic reaction
Useless positive acids, sulphonic acids, the processing of the organic catalysts such as non-metal kind and reuse method.
Background technology
Organic reaction has a very important status as the basis of chemical engineering industry in modern industry, organic reaction into
Row tends not to individually carry out, and needs to introduce the third medium, i.e. catalyst during the reaction.In numerous organic reaction processes
In, the application of the organic catalysts such as positive acids, sulphonic acids, non-metal kind is relatively broad.With the progress of reaction, the work of catalyst
Property continuously decreases, and catalyst inactivates in advance after some cycles are used or caused by misoperation, the activity of catalyst is not enough to
When meeting the needs of reaction, it is mainly shown as that the conversion ratio of raw material declines, the selectivity of purpose product declines, by-product increases
Several aspects need that catalyst is regenerated or replaced at this time.For being processed into for regenerated decaying catalyst can not be carried out
For the current a great problem that chemical enterprise faces mostly.Dead catalyst main component after inactivation is raw catalyst, Organic Ingredients,
Sour gas etc..
At present, it is that high-temperature process is carried out by rotary furnace for the processing method of such organic dead catalyst routine, makes residual
The material and supplies stayed are recycled at high temperature, using easily having remaining acidity in the catalyst waste slag after this process
Gas, not only penetrating odor is larger, and with certain corrosivity, still falls within dangerous solid waste, have to environment extremely strong
Pollution.
Invention content
Processing and recycling side in order to compensate for the shortcomings of the prior art, the present invention provides a kind of organic dead catalyst
Method solves to be widely used in processing and the recycling of the organic catalysts such as the useless positive acids, sulphonic acids, non-metal kind of organic reaction
Problem solves the problems, such as to still fall within the dead catalyst of solid dangerous waste object after conventional treatment, solves the work of decaying catalyst processing
Skill problem and the pollution problem to environment.
The present invention is achieved through the following technical solutions：
A kind of processing of organic dead catalyst and reuse method, step are as follows：
(1) organic dead catalyst is pressurizeed by nitrogen and is pressed into atomizer, and spraying enters rotary furnace and burns, and burns generation
Acid gas is absorbed through water caustic washing system, is neutralized；Atomisation pressure is controlled after nitrogen pressurization as 0.1-0.5MPa, temperature when rotary furnace burns
500-900 DEG C, burn 60s；
(2) step (1) products therefrom is cooled down, be delivered in reaction kettle, add water washing, after stirring 30-40 minutes, mistake
Filter, filter residue is after liquid caustic soda neutralizes, then washing filtering is three times, filtering, obtains washings and filter residue, and washings can be used for relieving haperacidity, filter residue
It can be directly used as making the raw material of water-coal-slurry；
(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；
(4) step (3) products therefrom be granulated, dried, being screened, magnetic separation, packaging, finished product carbon black, for again
It utilizes.
Step (1) burns the acid gas generated and absorbs, neutralizes through water caustic washing system.
Preferably, control atomisation pressure is 0.2-0.4MPa after the pressurization of step (1) nitrogen, temperature 600- when rotary furnace burns
800℃。
Preferably, the fuel used in step (1) rotary furnace is one kind in natural gas, coal gas, biogas.
Preferably, for washings obtained by step (2) for relieving haperacidity, filter residue is used as making the raw material of water-coal-slurry.
Preferably, the comminutor used when step (4) is granulated is a kind of type in wet granulator, squeezing comminutor.
Beneficial effects of the present invention：
A kind of processing of organic dead catalyst of the present invention and reuse method are solved in conventional dead catalyst treatment process
The recycling problem of product carbon, organic dead catalyst harmful substance after burning all absorbs in this method, it is not easy to have residual
Sour gas, water-coal-slurry or carbon black finished product, the closed processing of entire technical process whole process, anacidity is directly made using part
Property gas effusion.On the one hand the harmless treatment to organic dead catalyst is realized, being on the other hand changed into dangerous solid waste can
The product utilized while bringing benefits, solves the problems, such as environmental pollution, and economic benefit and social benefit are notable.
Specific embodiment
A kind of processing of the organic dead catalyst of embodiment 1 and reuse method, step are as follows：
(1) organic dead catalyst is pressurizeed by nitrogen and is pressed into atomizer, and spraying enters the rotary furnace (fuel in rotary furnace
For natural gas) it burns, the acid gas for burning generation is absorbed through water caustic washing system, is neutralized；Control atomisation pressure is after nitrogen pressurization
0.1MPa, 500 DEG C of temperature when rotary furnace burns burn 60s；
(2) step (1) products therefrom is cooled down, be delivered in reaction kettle, add water washing, after stirring 30 minutes, filtered, filter
Slag is after liquid caustic soda neutralizes, then washing filtering is three times, filtering, obtains washings and filter residue, and washings are used for relieving haperacidity, and filter residue is directly used as
Make the raw material of water-coal-slurry；
(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；
(4) step (3) products therefrom is granulated and (wet granulator is used during granulation), drying, screening, magnetic separation, packet
Dress, finished product carbon black, for reusing.
A kind of processing of the organic dead catalyst of embodiment 2 and reuse method, step are as follows：
(1) organic dead catalyst is pressurizeed by nitrogen and is pressed into atomizer, and spraying enters the rotary furnace (fuel in rotary furnace
For coal gas) it burns, the acid gas for burning generation is absorbed through water caustic washing system, is neutralized；Control atomisation pressure is after nitrogen pressurization
0.5MPa, 900 DEG C of temperature when rotary furnace burns burn 60s；
(2) step (1) products therefrom is cooled down, be delivered in reaction kettle, add water washing, stirring after forty minutes, is filtered, filter
Slag is after liquid caustic soda neutralizes, then washing filtering is three times, filtering, obtains washings and filter residue, and washings are used for relieving haperacidity, and filter residue is directly used as
Make the raw material of water-coal-slurry；
(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；
(4) step (3) products therefrom is granulated and (squeezing comminutor is used during granulation), drying, screening, magnetic separation, packet
Dress, finished product carbon black, for reusing.
A kind of processing of the organic dead catalyst of embodiment 3 and reuse method, step are as follows：
(1) organic dead catalyst is pressurizeed by nitrogen and is pressed into atomizer, and spraying enters the rotary furnace (fuel in rotary furnace
For natural gas) it burns, the acid gas for burning generation is absorbed through water caustic washing system, is neutralized；Control atomisation pressure is after nitrogen pressurization
0.2MPa, 600 DEG C of temperature when rotary furnace burns burn 60s；
(2) step (1) products therefrom is cooled down, be delivered in reaction kettle, add water washing, after stirring 33 minutes, filtered, filter
Slag is after liquid caustic soda neutralizes, then washing filtering is three times, filtering, obtains washings and filter residue, and washings are used for relieving haperacidity, and filter residue is directly used as
Make the raw material of water-coal-slurry；
(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；
(4) step (3) products therefrom is granulated and (wet granulator is used during granulation), drying, screening, magnetic separation, packet
Dress, finished product carbon black, for reusing.
A kind of processing of the organic dead catalyst of embodiment 4 and reuse method, step are as follows：
(1) organic dead catalyst is pressurizeed by nitrogen and is pressed into atomizer, and spraying enters the rotary furnace (fuel in rotary furnace
For coal gas) it burns, the acid gas for burning generation is absorbed through water caustic washing system, is neutralized；Control atomisation pressure is after nitrogen pressurization
0.4MPa, 800 DEG C of temperature when rotary furnace burns burn 60s；
(2) step (1) products therefrom is cooled down, be delivered in reaction kettle, add water washing, after stirring 37 minutes, filtered, filter
Slag is after liquid caustic soda neutralizes, then washing filtering is three times, filtering, obtains washings and filter residue, and washings are used for relieving haperacidity, and filter residue is directly used as
Make the raw material of water-coal-slurry；
(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；
(4) step (3) products therefrom is granulated and (squeezing comminutor is used during granulation), drying, screening, magnetic separation, packet
Dress, finished product carbon black, for reusing.
A kind of processing of the organic dead catalyst of embodiment 5 and reuse method, step are as follows：
(1) organic dead catalyst is pressurizeed by nitrogen and is pressed into atomizer, and spraying enters the rotary furnace (fuel in rotary furnace
For natural gas) it burns, the acid gas for burning generation is absorbed through water caustic washing system, is neutralized；Control atomisation pressure is after nitrogen pressurization
0.3MPa, 700 DEG C of temperature when rotary furnace burns burn 60s；
(2) step (1) products therefrom is cooled down, be delivered in reaction kettle, add water washing, after stirring 35 minutes, filtered, filter
Slag is after liquid caustic soda neutralizes, then washing filtering is three times, filtering, obtains washings and filter residue, and washings are used for relieving haperacidity, and filter residue is directly used as
Make the raw material of water-coal-slurry；
(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；
(4) step (3) products therefrom is granulated and (wet granulator is used during granulation), drying, screening, magnetic separation, packet
Dress, finished product carbon black, for reusing.
A kind of processing of the organic dead catalyst of embodiment 6 and reuse method, step are as follows：
(1) organic dead catalyst is pressurizeed by nitrogen and is pressed into atomizer, and spraying enters the rotary furnace (fuel in rotary furnace
For coal gas) it burns, the acid gas for burning generation is absorbed through water caustic washing system, is neutralized；Control atomisation pressure is after nitrogen pressurization
0.3MPa, 700 DEG C of temperature when rotary furnace burns burn 60s；
(2) step (1) products therefrom is cooled down, be delivered in reaction kettle, add water washing, after stirring 35 minutes, filtered, filter
Slag is after liquid caustic soda neutralizes, then washing filtering is three times, filtering, obtains washings and filter residue, and washings are used for relieving haperacidity, and filter residue is directly used as
Make the raw material of water-coal-slurry；
(3) filter residue obtained by step (2) is ground, crosses 325 mesh sieve；Sieving rate is 99.9%；
(4) step (3) products therefrom is granulated and (squeezing comminutor is used during granulation), drying, screening, magnetic separation, packet
Dress, finished product carbon black, for reusing.
Test example：In order to verify the effect of a kind of processing of organic dead catalyst of the present invention and reuse method, the present invention
People has done contrast test, is specifically divided into control group and experimental group.
Used organic dead catalyst in 3 kinds of chemical laboratories is collected, respectively for the useless positive acids of organic reaction
Organic catalyst, useless sulphonic acids organic catalyst, useless non-metal kind organic catalyst, respectively collect 30g.It is useless by what is be collected at random
Positive acids organic catalyst, useless sulphonic acids organic catalyst, useless non-metal kind organic catalyst are divided evenly into three parts, every portion
Point it is 10g, number is positive acids A, positive acids B, positive acids C, sulphonic acids A, sulphonic acids B, sulphonic acids C, non-metal kind A, non-
Metal class B, non-metal kind C, sealing are placed.
Wherein, positive acids A, sulphonic acids A, non-metal kind A, using traditional treatment method, directly will respectively for control group
It is burned, and measures the main component index of product obtained after burning, and specific data are shown in Table 1.
Positive acids B, positive acids C, sulphonic acids B, sulphonic acids C, non-metal kind B, non-metal kind C are adopted respectively for experimental group
It is handled with the method for 1-6 of the embodiment of the present invention, measures the main component index of final products, specific data are shown in Table 1.
Table 1：Main component index of the different types of organic dead catalyst after different disposal
By table 1 as it can be seen that either to the positive acids organic catalyst that gives up still to useless sulphonic acids organic catalyst or the non-gold that gives up
Belong to class organic catalyst processing, using the iodine absorption value of the products therefrom after processing method of the present invention, CTAB adsorption specific surface areas,
300% stress at definite elongation, oil factor are obviously higher than all index values using products therefrom after traditional treatment method；Meanwhile it adopts
It is significantly lower than using traditional treatment method with the content of ashes and impurity content of the products therefrom after processing method of the present invention
All index contents of products therefrom afterwards.Obviously the performance of the processing method products therefrom of the organic dead catalyst of the present invention is more excellent
It is good, the grade quality higher of gained carbon black, so a kind of processing of organic dead catalyst of the present invention and reuse method are more excellent
Useless ortho-acid, sulfonic acid, non-metallic organocatalyst processing and recycle project.
Claims (6)
1. processing and the reuse method of a kind of organic dead catalyst, it is characterized in that：Step is as follows：
（1）Organic dead catalyst is pressed into atomizer by nitrogen pressurization, spraying enters in rotary furnace, burns；Atomisation pressure
For 0.1-0.5MPa, temperature is 500-900 DEG C when rotary furnace burns, and the burning time is 60s；
（2）By step（1）It after products therefrom cooling, is delivered in reaction kettle, adds water, after stirring 30-40 minutes, filtering, filter residue
After liquid caustic soda neutralizes, then washing filtering is three times, obtains washings and filter residue；
（3）By step（2）Gained filter residue is ground, and crosses 325 mesh sieve；Sieving rate is 99.9%；
（4）By step（3）Products therefrom is granulated, is dried, being screened, magnetic separation, packaging, finished product carbon black, for reusing；
Organic dead catalyst is the useless positive acids organic catalyst for organic reaction, useless sulphonic acids organic catalyst, useless
Any one in non-metal kind organic catalyst.
2. processing and the reuse method of a kind of organic dead catalyst according to claim 1, it is characterized in that：Step（1）
The acid gas generated is burned to absorb, neutralize through water caustic washing system.
3. processing and the reuse method of a kind of organic dead catalyst according to claim 1, it is characterized in that：Step（1）
Atomisation pressure is controlled after nitrogen pressurization as 0.2-0.4MPa, 600-800 DEG C of temperature when rotary furnace burns.
4. processing and the reuse method of a kind of organic dead catalyst according to claim 1, it is characterized in that：Step（1）
The fuel used in rotary furnace is one kind in natural gas, coal gas, biogas.
5. processing and the reuse method of a kind of organic dead catalyst according to claim 1, it is characterized in that：Step（2）
Gained washings are used for relieving haperacidity, and filter residue is used as making the raw material of water-coal-slurry.
6. processing and the reuse method of a kind of organic dead catalyst according to claim 1, it is characterized in that：Step（4）
The comminutor used during granulation is a kind of type in wet granulator, squeezing comminutor.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102335668A (en) * | 2010-07-19 | 2012-02-01 | 车磊 | Method for treating industrial hazardous wastes containing organic solvent |
| CN204704822U (en) * | 2015-06-19 | 2015-10-14 | 山东华安新材料有限公司 | For the treatment system of the dead catalyst fluosulfonic acid that alkene or alkynes react |
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2016
- 2016-08-31 CN CN201610792396.7A patent/CN106433227B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102335668A (en) * | 2010-07-19 | 2012-02-01 | 车磊 | Method for treating industrial hazardous wastes containing organic solvent |
| CN204704822U (en) * | 2015-06-19 | 2015-10-14 | 山东华安新材料有限公司 | For the treatment system of the dead catalyst fluosulfonic acid that alkene or alkynes react |
Non-Patent Citations (1)
| Title |
|---|
| "废催化剂回收利用现状及对策";王世芬 等;《能源研究与管理》;20150615;第2卷;第118-121页 * |
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