CN107952260A - Method for extracting and recovering chemicals from carbon black after cracking waste rubber - Google Patents
Method for extracting and recovering chemicals from carbon black after cracking waste rubber Download PDFInfo
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- CN107952260A CN107952260A CN201611022120.7A CN201611022120A CN107952260A CN 107952260 A CN107952260 A CN 107952260A CN 201611022120 A CN201611022120 A CN 201611022120A CN 107952260 A CN107952260 A CN 107952260A
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- 238000000034 method Methods 0.000 title claims abstract description 141
- 239000006229 carbon black Substances 0.000 title claims abstract description 55
- 238000005336 cracking Methods 0.000 title claims abstract description 25
- 239000002699 waste material Substances 0.000 title claims abstract description 8
- 239000000126 substance Substances 0.000 title abstract description 24
- 230000018044 dehydration Effects 0.000 claims abstract description 29
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 21
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000012545 processing Methods 0.000 claims description 115
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 68
- 239000013049 sediment Substances 0.000 claims description 47
- 238000004064 recycling Methods 0.000 claims description 32
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 30
- 238000000605 extraction Methods 0.000 claims description 22
- 238000011084 recovery Methods 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910000765 intermetallic Inorganic materials 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- 238000001311 chemical methods and process Methods 0.000 claims description 17
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 15
- 238000002425 crystallisation Methods 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- 238000000197 pyrolysis Methods 0.000 claims description 14
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 12
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 12
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 11
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 10
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 9
- 229960001763 zinc sulfate Drugs 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical group OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 230000035939 shock Effects 0.000 claims 1
- ORVGYTXFUWTWDM-UHFFFAOYSA-N silicic acid;sodium Chemical compound [Na].O[Si](O)(O)O ORVGYTXFUWTWDM-UHFFFAOYSA-N 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 9
- 239000003513 alkali Substances 0.000 abstract description 3
- 239000011259 mixed solution Substances 0.000 abstract 4
- 239000002244 precipitate Substances 0.000 abstract 4
- 150000002736 metal compounds Chemical class 0.000 abstract 2
- 235000019241 carbon black Nutrition 0.000 description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 37
- 239000002956 ash Substances 0.000 description 26
- 238000005406 washing Methods 0.000 description 19
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 14
- 229910052911 sodium silicate Inorganic materials 0.000 description 11
- 239000004115 Sodium Silicate Substances 0.000 description 10
- 235000019795 sodium metasilicate Nutrition 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000000292 calcium oxide Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229920002472 Starch Polymers 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000002738 chelating agent Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 235000019353 potassium silicate Nutrition 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000001465 metallisation Methods 0.000 description 3
- 238000005201 scrubbing Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 239000011686 zinc sulphate Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- 241000565357 Fraxinus nigra Species 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910014779 CaAl4 Inorganic materials 0.000 description 1
- 229910014813 CaC2 Inorganic materials 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 229910007426 ZnC2 Inorganic materials 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GSOLWAFGMNOBSY-UHFFFAOYSA-N cobalt Chemical compound [Co][Co][Co][Co][Co][Co][Co][Co] GSOLWAFGMNOBSY-UHFFFAOYSA-N 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 description 1
- AMFIJXSMYBKJQV-UHFFFAOYSA-L cobalt(2+);octadecanoate Chemical compound [Co+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AMFIJXSMYBKJQV-UHFFFAOYSA-L 0.000 description 1
- BGORGFZEVHFAQU-UHFFFAOYSA-L cobalt(2+);sulfate;hydrate Chemical compound O.[Co+2].[O-]S([O-])(=O)=O BGORGFZEVHFAQU-UHFFFAOYSA-L 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000446 fuel Substances 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
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 229910001387 inorganic aluminate Inorganic materials 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- HNBFUFIYQWYCDM-UHFFFAOYSA-N oxygen(2-) sulfane titanium(4+) Chemical compound [O--].[O--].S.[Ti+4] HNBFUFIYQWYCDM-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/06—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/482—Preparation from used rubber products, e.g. tyres
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/487—Separation; Recovery
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a method for extracting and recovering chemicals from carbon black after cracking waste rubber, which at least comprises the following steps: providing a cracking solid, wherein the cracking solid is obtained by cracking waste rubber; providing an acid solution, putting the acid solution and the cracked solid into a stirring device, and performing a first stirring process to generate a first mixed solution; separating the first mixed solution into a first solution and a first precipitate by a first separation process, and obtaining a first metal compound by the first solution by a first dehydration process; providing an alkali solution, putting the alkali solution and the first precipitate into a stirring device, and performing a second stirring process to generate a second mixed solution; separating the second mixed solution into a second solution and a second precipitate by a second separation process, and obtaining a second metal compound from the second solution by a second dehydration process; and subjecting the second precipitate to a third dehydration process to obtain carbon black.
Description
Technical field
The present invention is related to a kind of extraction and recovery chemical processes of carbon black after scrap rubber cracking, and particularly a kind of recycling is useless
Sulfur dioxide caused by rubber cracking processing procedure is recycled with recycling high level chemicals, and improves the scrap rubber cracking of carbon black quality
The extractive recovery method of carbon black afterwards.
Background technology
Global people's exchange is frequent now, and exchanging frequent result causes the people of all parts of the world constantly to be moved toward various regions
It is dynamic, and greatly increase the demand of the vehicles, no matter take a flight, vehicle etc. all needs to use tire, also make making for tire
Dosage greatly increases, the increase of the usage amount of tire, and causes because that need to eliminate the tire quantity changed using consume also just greatly
Increase, and tire is rubber, therefore, the recycle and reuse of scrap rubber becomes an important problem.
The recycle and reuse major technique of scrap rubber is to crack scrap rubber and extract recyclable composition, scrap rubber
Meeting output methane gas in cracking process, and the heat source fuel using methane gas recycling as pyrolysis furnace cracking scrap rubber.Cause
Sulphur must be just added during for refining rubber, so as to the physical characteristic of reinforcing rubber, and meets commercial specification, so
For scrap rubber after cracking, sulphur is oxidized into sulfur dioxide through burning（SO2）Gas.
In order to remove air pollution factor sulfur dioxide, most straightforward procedure be exactly by this sulfur dioxide water after burning in
Wash and intercept in scrubbing tower, sulfuric acid solution is formed during sulfur dioxide dissolves easily in water in scrubbing tower, then this sulfuric acid solution
It can discharge after need to being neutralized with lye or further be handled in uniting into wastewater treatment, form the waste of resource, also increased place
Manage cost and the burden of environment.
And carbon black is the target mainly recycled in technology today in rubber component, carbon black is the reinforcing material of rubber composition
Material, carbon black can constantly be recycled repetition in theory and be reused due to its excellent stability, but due in the formula of rubber still
Other metals and nonmetal oxide need to be added or compound can be only achieved the requirement that general business uses basic specification, it is such
Material can not separate in scrap rubber cracks program and from solid carbon black, or the pass because of Pintsch process and makes portion
Part material has also assisted in chemical reaction, and produces extra ashes, i.e., the ash of so-called carbon black.Therefore, the purity of carbon black is caused
It is bad, generally about contain 10 ~ 20% ash, influence to make an addition to the strengthening action of rubber after recycling carbon black, greatly reduce recycling
Carbon black also causes the industry development of scrap rubber cracking recycling to be extremely limited in the applicability and its marketability of rubber.
Technology today mainly carries out pickling processing procedure using acid solution and chelating agent to carbon black, with acid solution by carbon black
Ash chemically reacts with it, and is separated with chelating agent with the metal ion-chelant in the ash of carbon black, to reduce the ash of carbon black
Therefore the major technique of part, still, because additionally to add chelating agent, also adds processing cost and the burden of environment.
The content of the invention
In view of this, to solve the above problems, the present invention provides a kind of extraction and recovery chemistry of carbon black after scrap rubber cracking
Product method, recycling scrap rubber crack sulfur dioxide caused by processing procedure and recycle, and without extra addition chelating agent, effectively reduce
The ash of carbon black and improve carbon black quality, recycle high level metal extractive recovery method.
The high level metal that the present invention is recycled can be ZnS, CaCO3、Al2Si2O5、Zn3O(SiO4)2ZnAlSiO、ZnSO4、
CaO2、ZnSO3、CaAl4O7、ZnC2O4、CaC2O4、CaO、AlO4C、CSiO2、(Al1.98Fe0.2)SiO5Deng metallic compound.
The extraction and recovery chemical processes of carbon black after being cracked disclosed herein scrap rubber, it includes at least the following steps：
A pyrolysis solid thing is provided, which obtains for scrap rubber through cracking；One acid solution is provided, which is split with this
Solution solids is inserted in agitating device, is carried out the first stirring processing procedure, is produced one first mixed liquor；By first mixed liquor through first
Separate processing procedure and be separated into one first solution and one first sediment, which obtains the first gold medal through the first dehydration processing procedure
Belong to compound；One aqueous slkali is provided, the aqueous slkali and first sediment are inserted in agitating device, carries out the second stirring system
Journey, produces one second mixed liquor；Second mixed liquor is separated into one second solution and sunk with one second through the second separation processing procedure
Starch, second solution obtain the second metallic compound through the second dehydration processing procedure；And second sediment is taken off through the 3rd
Water processing procedure and obtain carbon black.
The present invention can make the chemistry of recycling carbon black, physical property closer to commercial carbon blacks N-330 standard, to rubber cracking
And carbon black, using for dealer, the present invention even more such as has a long-felt need satisfied.
It is the thing that part kills two birds with one stone that the present invention carries out the processing of carbon black ash using the sulfuric acid solution of scrubbing tower recycling, without volume
Outer lye neutralizes the acid of output and can remove in carbon black contained ash, improves the quality of recycling carbon black, and recyclable high level
Metal, the real technology for belonging to environmental protection and having economic value again.
Brief description of the drawings
Fig. 1 is the flow chart according to the embodiment of the present invention.
【Symbol description】
10 pyrolysis solid things；
11 acid solutions；
12 first stirring processing procedures；
13 first mixed liquors；
14 first separation processing procedures；
15 first solution；
151 first dehydration processing procedures；
152 first metallic compounds；
16 first sediments；
21 aqueous slkalis；
22 second stirring processing procedures；
23 second mixed liquors；
24 second separation processing procedures；
25 second solution；
251 second dehydration processing procedures；
252 second metallic compounds；
26 second sediments；
261 the 3rd dehydration processing procedures；
262 carbon blacks.
Embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, so that those skilled in the art can be with
It is better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
Below, it will be explained in the extraction and recovery chemicals of carbon black after scrap rubber according to embodiments of the present invention cracks
Method.
Please be shown in Figure 1, Fig. 1 is the flow chart according to the embodiment of the present invention, and disclosed herein scrap rubber cracking
The extraction and recovery chemical processes of carbon black afterwards, it can include at least the following steps：Pyrolysis solid thing 10, pyrolysis solid thing 10 are provided
Obtained for scrap rubber through cracking；Acid solution 11 is provided, acid solution 11 and pyrolysis solid thing 10 are inserted in agitating device, carries out the
One stirring processing procedure 12, produces the first mixed liquor 13；First mixed liquor 13 is separated into the first solution through the first separation processing procedure 14
15 and first sediment 16, the first solution 15 obtain the first metallic compound 152 through the first dehydration processing procedure 151；Alkali soluble is provided
Liquid 21,21 and first sediment 16 of aqueous slkali is inserted in agitating device, is carried out the second stirring processing procedure 22, is produced the second mixed liquor
23；Second mixed liquor 23 is separated into the second solution 25 and the second sediment 26 through the second separation processing procedure 24, the second solution 25
The second metallic compound 252 is obtained through the second dehydration processing procedure 251；And by the second sediment 26 through the 3rd dehydration processing procedure 261
And obtain carbon black 262.Wherein, scrap rubber can be recycling rubber, rubber can be rubber made by tire, shock-absorbing
Device, packing ring, medical equipment, sole, gloves or toy；Acid solution 11 may include to be selected from by sulfuric acid solution, hydrochloric acid solution, nitric acid
The group that solution, phosphoric acid solution, oxalic acid solution, formic acid solution, acetic acid solution are formed with crossing solution chlorate, it is most preferably adjustable to be assigned to
PH-value（pH）1.0 or less；Also device in Gas burning of the scrap rubber through cracking processing procedure output can be produced sulfur dioxide, titanium dioxide
Sulphur is reacted into sulfuric acid solution through waste reduction device and water；First stirring processing procedure 12 can carry out 0.5 it is small when more than, most preferably can be 0.5 ~ 3
Hour, in room temperature or 50 ~ 90 DEG C can be gradually heating to；First separation processing procedure 14 can be selected from by extraction processing procedure, precipitation processing procedure with
The group that filtering process is formed；First dehydration processing procedure 151 can be for selected from by drying processing procedure, evaporative crystallization and air-dried processing procedure institute group
Into group；First metallic compound 152 may include selected from the group being made of zinc sulfate, nickel sulfate, calcium sulfate and cobaltous sulfate
Group；Aqueous slkali 21 may include to be also known as causticity selected from the group being made of sodium hydroxide solution and ammonium hydroxide, sodium hydroxide solution
Aqueous slkali；Second stirring processing procedure 22 can carry out 0.5 it is small when more than, most preferably can be 0.5 ~ 6 it is small when, in room temperature or can be gradually heating to
50~90℃；Second separation processing procedure 24 can be for selected from the group being made of extraction processing procedure, precipitation processing procedure with filtering process；Second
Dehydration processing procedure 251 can be for selected from the group being made of drying processing procedure, evaporative crystallization with air-dried processing procedure；Second metallic compound
252 can be sodium metasilicate；3rd dehydration processing procedure 261 can be by selected from being made of drying processing procedure, centrifugal dehydration processing procedure and air-dried processing procedure
Group.
Furtherly, the method selected from the group being made of drying processing procedure, evaporative crystallization with air-dried processing procedure can also be used
First sediment 16 is dried again.
Furtherly, disclosed herein method, recyclable high level chemicals, for example, the first metallic compound 152,
Second metallic compound 252 and carbon black 262.
Wherein, the first metallic compound 152 may include selected from the group being made of cobaltous sulfate, nickel sulfate and zinc sulfate,
It is acted on ash and acid solution 11, and wherein ash can include zinc oxide, zinc, nickel oxide, nickel, calcium oxide or stearic acid
Cobalt（Cobaltstearate）Deng metallic compound.
Zinc oxide and sulfuric acid solution act on, such as following chemical formula 1,
[chemical formula 1]
ZnO + H2SO4 → ZnSO4 + H2O
Produce zinc sulfate.
Zinc and sulfuric acid solution act on, such as following chemical formula 2,
[chemical formula 2]
Zn + H2SO4 → ZnSO4 + H2
Produce zinc sulfate.
Nickel oxide and sulfuric acid solution act on, such as following chemical formula 3,
[chemical formula 3]
NiO + H2SO4 → NiSO4 + H2O
Produce nickel sulfate.
Nickel and sulfuric acid solution act on, such as following chemical formula 4,
[chemical formula 4]
Ni + H2SO4 → NiSO4 + H2
Produce nickel sulfate.
Calcium oxide and sulfuric acid solution act on, such as following chemical formula 5,
[chemical formula 5]
CaO + H2SO4 → CaSO4 + H2O
Produce calcium sulfate.
Cobaltous octadecanate and sulfuric acid solution act on, such as following chemical formula 6,
[chemical formula 6]
C36H70CoO4 + H2SO4 → CoSO4·7H2O + 2C18H36O2
Cobalt sulfate hydrate is produced, can heat and be dehydrated into cobaltous sulfate.
Wherein, the second metallic compound 252 can be sodium metasilicate, it is to be acted on ash and aqueous slkali 21, wherein ash
Part can also include the nonmetal oxides such as silica.
Silica and aqueous slkali act on, such as following chemical formula 7,
[chemical formula 7]
SiO2 + 2NaOH → Na2SiO3 + H2O
Produce sodium metasilicate, also known as waterglass.
The present invention discloses again can utilize the waste reduction equipment for washing tower cracked in processing procedure, and processing procedure output sulfur dioxide is washed
Tower, by sulfur dioxide with forming sulfurous acid under washing and being hydrolyzed into sulfuric acid solution rapidly again, such as following chemical formula 9,
[chemical formula 9]
SO2 + 2H2O → H2SO4 + 2H+
And by the sulfuric acid solution of recycling collect to acidifying groove in it is spare, foregoing sulfuric acid solution can be become（Acid solution）Source.
Illustrate the present invention by means of following embodiments, but the present invention is not limited thereto,
Embodiment 1
50 g of pyrolysis solid thing is provided, measurement there are about 15.45% ash, it is ground recycling carbon black, for recycling
Scrap rubber is obtained through general cracking processing procedure.
Acid solution is provided, it is configured to the sulfuric acid of 0.1N to provide 1 liter of pure water, about 10 g of the concentrated sulfuric acid of addition
Solution.
By sulfuric acid solution（Acid solution）With recycling carbon black（Pyrolysis solid thing）Slowly it is placed into agitating device, makes recycling carbon
It is black to be completely immersed in sulfuric acid solution, and be persistently stirred 2 it is small when, in room temperature be gradually heating to 70 DEG C（First stirring system
Journey）, produce the first mixed liquor.
Stop stirring, by the first mixed liquor through extracting processing procedure, precipitation processing procedure and filtering process（First separation processing procedure）And divide
From into the first sediment and the first solution.
With 1 ~ 3 times of first sediment of pure water of the first sediment volume, the liquid after clear water washing is first heavy
Starch cleaning solution.
By the first sediment undergoes washing liquid and the first solution drying processing procedure, evaporative crystallization and air-dried processing procedure（First dehydration system
Journey）And obtain zinc sulfate, nickel sulfate, calcium sulfate and cobaltous sulfate of the embodiment of the present invention 1 etc.（First metallic compound）, it is height
The chemicals of value.
Aqueous slkali is provided, sodium hydroxide is configured to 0.1N, 1 liter of sodium hydroxide solution.
By sodium hydroxide solution（Aqueous slkali）Inserted with the first sediment in agitating device, be persistently stirred 5 it is small when, in
Room temperature is gradually heating to 50 DEG C（Second stirring processing procedure）, produce the second mixed liquor.
Stop stirring, by the second mixed liquor through extracting processing procedure, precipitation processing procedure and filtering process（Second separation processing procedure）And divide
From into the second sediment and the second solution.
With 1 ~ 3 times of second sediment of pure water of the second sediment volume, after again by the second sediment drying system
Journey, evaporative crystallization and air-dried processing procedure（3rd dehydration processing procedure）And obtain the carbon black of the embodiment of the present invention 1.
Liquid after clear water washing is the second sediment undergoes washing liquid, by the second sediment undergoes washing liquid and the second solution through drying
Drying journey, evaporative crystallization and air-dried processing procedure（Second dehydration processing procedure）And obtain the sodium metasilicate of the embodiment of the present invention 1（Second metallization
Compound）Deng sodium metasilicate is also known as waterglass.
The carbon black of the embodiment of the present invention 1 is measured, its ash is 6.35%, that is to say, that is down to by original ash 15.45%
6.35%, it was demonstrated that the embodiment of the present invention 1 can obtain the recycling carbon black that ash is low, purity is high.
Embodiment 2
100 g of pyrolysis solid thing is provided, measurement there are about 15.45% ash, it is ground recycling carbon black, for recycling
Scrap rubber through obtained by general cracking processing procedure.
Acid solution is provided, it is provides 1 liter of pure water, about 100 g of the concentrated sulfuric acid of addition, and the sulfuric acid for being configured to 1N is molten
Liquid.
By sulfuric acid solution（Acid solution）With recycling carbon black（Pyrolysis solid thing）Slowly it is placed into agitating device, makes recycling carbon
It is black to be completely immersed in sulfuric acid solution, and be persistently stirred 1 it is small when, in room temperature be gradually heating to 80 DEG C（First stirring system
Journey）, produce the first mixed liquor.
Stop stirring, by the first mixed liquor through extracting processing procedure, precipitation processing procedure and filtering process（First separation processing procedure）And divide
From into the first sediment and the first solution.
With 1 ~ 3 times of first sediment of pure water of the first sediment volume, the liquid after clear water washing is first heavy
Starch cleaning solution.
By the first sediment undergoes washing liquid and the first solution drying processing procedure, evaporative crystallization and air-dried processing procedure（First dehydration system
Journey）And obtain zinc sulfate, nickel sulfate, calcium sulfate and cobaltous sulfate of the embodiment of the present invention 2 etc.（First metallic compound）, it is height
The chemicals of value.
Aqueous slkali is provided, sodium hydroxide is configured to 1N, 1 liter of sodium hydroxide solution.
By sodium hydroxide solution（Aqueous slkali）Inserted with the first sediment in agitating device, be persistently stirred 2 it is small when, in
Room temperature is gradually heating to 70 DEG C（Second stirring processing procedure）, produce the second mixed liquor.
Stop stirring, by the second mixed liquor through extracting processing procedure, precipitation processing procedure and filtering process（Second separation processing procedure）And divide
From into the second sediment and the second solution.
With 1 ~ 3 times of second sediment of pure water of the second sediment volume, after again by the second sediment drying system
Journey, evaporative crystallization and air-dried processing procedure（3rd dehydration processing procedure）And obtain the carbon black of the embodiment of the present invention 2.
Liquid after clear water washing is the second sediment undergoes washing liquid, by the second sediment undergoes washing liquid and the second solution through drying
Drying journey, evaporative crystallization and air-dried processing procedure（Second dehydration processing procedure）And obtain the sodium metasilicate of the embodiment of the present invention 2（Second metallization
Compound）Deng sodium metasilicate is also known as waterglass.
The carbon black of the embodiment of the present invention 2 is measured, its ash is 4.04%, that is to say, that is down to by original ash 15.45%
4.04%, it was demonstrated that the embodiment of the present invention 2 can obtain the recycling carbon black that ash is low, purity is high.
Embodiment 3
50 g of pyrolysis solid thing is provided, measurement there are about 15.45% ash, it is ground recycling carbon black, for recycling
Scrap rubber is through obtained by general cracking processing procedure.
Acid solution is provided, using the waste reduction equipment for washing tower cracked in processing procedure, by the washed tower of processing procedure output sulfur dioxide,
By sulfur dioxide with being hydrolyzed into sulfuric acid solution under washing, and the sulfuric acid solution of recycling is collected into acidifying groove, and be recycling
Sulfuric acid solution, by the sulfuric acid solution and the concentrated sulfuric acid of recycling, is configured to 1N, 1 liter of sulfuric acid solution.
By sulfuric acid solution（Acid solution）With recycling carbon black（Pyrolysis solid thing）Slowly it is placed into agitating device, makes recycling carbon
It is black to be completely immersed in sulfuric acid solution, and be persistently stirred 3 it is small when, in room temperature be gradually heating to 90 DEG C（First stirring system
Journey）, produce the first mixed liquor.
Stop stirring, by the first mixed liquor through extracting processing procedure, precipitation processing procedure and filtering process（First separation processing procedure）And divide
From into the first sediment and the first solution.
With 1 ~ 3 times of first sediment of pure water of the first sediment volume, the liquid after clear water washing is first heavy
Starch cleaning solution.
By the first sediment undergoes washing liquid and the first solution drying processing procedure, evaporative crystallization and air-dried processing procedure（First dehydration system
Journey）And obtain zinc sulfate, nickel sulfate, calcium sulfate and cobaltous sulfate of the embodiment of the present invention 3 etc.（First metallic compound）, it is height
The chemicals of value.
Aqueous slkali is provided, sodium hydroxide is configured to 1N, 1 liter of sodium hydroxide solution.
By sodium hydroxide solution（Aqueous slkali）Inserted with the first sediment in agitating device, be persistently stirred 5 it is small when, in
Room temperature is gradually heating to 80 DEG C（Second stirring processing procedure）, produce the second mixed liquor.
Stop stirring, by the second mixed liquor through extracting processing procedure, precipitation processing procedure and filtering process（Second separation processing procedure）And divide
From into the second sediment and the second solution.
With 1 ~ 3 times of second sediment of pure water of the second sediment volume, after again by the second sediment drying system
Journey, evaporative crystallization and air-dried processing procedure（3rd dehydration processing procedure）And obtain the carbon black of the embodiment of the present invention 3.
Liquid after clear water washing is the second sediment undergoes washing liquid, by the second sediment undergoes washing liquid and the second solution through drying
Drying journey, evaporative crystallization and air-dried processing procedure（Second dehydration processing procedure）And obtain the sodium metasilicate of the embodiment of the present invention 3（Second metallization
Compound）Deng sodium metasilicate is also known as waterglass.
The carbon black of the embodiment of the present invention 3 is measured, its ash is 3.11%, that is to say, that is down to by original ash 15.45%
3.11%, it was demonstrated that the embodiment of the present invention 3 can obtain the recycling carbon black that ash is low, purity is high.
The according to embodiments of the present invention 1, embodiment of the present invention 2 proves to learn with the embodiment of the present invention 3, and the present invention asks can general
Ash in carbon black effectively extracts, and one conveniently obtains the recycling carbon black that ash is low, purity is high, and script is influenced carbon black product
The ash of matter extracts the high-valued product such as zinc sulfate, nickel sulfate, calcium sulfate, cobaltous sulfate and sodium metasilicate, and recycles sulfur dioxide
Recycle, to have environmental protection, high-quality and the technology of high value concurrently.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
Enclose not limited to this.The equivalent substitute or conversion that those skilled in the art are made on the basis of the present invention, in the present invention
Protection domain within.Protection scope of the present invention is subject to claims.
Claims (13)
1. the extraction and recovery chemical processes of carbon black after a kind of scrap rubber cracking, it is characterised in that including at least the following steps：
A pyrolysis solid thing is provided, which obtains for scrap rubber through cracking；
One acid solution is provided, the acid solution and the pyrolysis solid thing are inserted in agitating device, the first stirring processing procedure is carried out, produces
One first mixed liquor；
First mixed liquor is separated into one first solution and one first sediment through the first separation processing procedure, first solution warp
First is dehydrated processing procedure and obtains the first metallic compound；
One aqueous slkali is provided, the aqueous slkali and first sediment are inserted in agitating device, the second stirring processing procedure is carried out, produces
One second mixed liquor；
Second mixed liquor is separated into one second solution and one second sediment through the second separation processing procedure, second solution warp
Second is dehydrated processing procedure and obtains the second metallic compound；And
Second sediment is obtained into carbon black through the 3rd dehydration processing procedure.
2. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that the scrap rubber is the rubber system of recycling
Product.
3. extraction and recovery chemical processes as claimed in claim 2, it is characterised in that the rubber is made by rubber
Tire, shock absorbing apparatus, packing ring, medical equipment, sole, gloves or toy.
4. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that the acid solution includes being selected from molten by sulfuric acid
Liquid, hydrochloric acid solution, salpeter solution, phosphoric acid solution, oxalic acid solution, formic acid solution, acetic acid solution are formed with crossing solution chlorate
Group.
5. extraction and recovery chemical processes as claimed in claim 4, it is characterised in that scrap rubber is produced two through cracking processing procedure
Sulfur oxide, sulfur dioxide are reacted into the sulfuric acid solution through waste reduction device and water.
6. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that the first separation processing procedure is selected from by extracting
The group for taking processing procedure, precipitation processing procedure to be formed with filtering process.
7. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that the first dehydration processing procedure is selected from by drying
The group that drying journey, evaporative crystallization are formed with air-dried processing procedure.
8. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that first metallic compound includes being selected from
The group being made of zinc sulfate, nickel sulfate, calcium sulfate and cobaltous sulfate.
9. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that the aqueous slkali includes being selected from by hydroxide
The group that sodium solution is formed with ammonium hydroxide.
10. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that this second separation processing procedure be selected from by
The group that extraction processing procedure, precipitation processing procedure are formed with filtering process.
11. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that this second dehydration processing procedure be selected from by
The group that drying processing procedure, evaporative crystallization are formed with air-dried processing procedure.
12. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that second metallic compound is silicic acid
Sodium.
13. extraction and recovery chemical processes as claimed in claim 1, it is characterised in that the 3rd dehydration processing procedure be selected from by
The group that drying processing procedure, centrifugal dehydration processing procedure are formed with air-dried processing procedure.
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| TW105133260 | 2016-10-14 | ||
| TW105133260A TW201813923A (en) | 2016-10-14 | 2016-10-14 | Method for recovering and extracting chemical products from carbon black after pyrolysis of waste rubber capable of recycling sulfur dioxide to reuse high-value chemicals |
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| CN109705635A (en) * | 2018-11-28 | 2019-05-03 | 昆明理工大学 | A kind of damaged tire cracking black carbon deliming and the method for ZnO recycling |
| CN110878148A (en) * | 2019-11-19 | 2020-03-13 | 珠海格力绿色再生资源有限公司 | Method for modifying pyrolysis carbon black |
| CN113694891A (en) * | 2021-08-26 | 2021-11-26 | 华侨大学 | Method for preparing carbon black adsorbing material based on 3D printing |
| CN115446096A (en) * | 2022-08-29 | 2022-12-09 | 北京科技大学 | Method for preparing blast furnace injection fuel and zinc carbonate by cracking waste tire carbon black |
| GB2622610A (en) * | 2022-09-22 | 2024-03-27 | Ppp Portglenone Ltd | A method for obtaining carbon black, the carbon black obtained therefrom and the use thereof |
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| CN109705635A (en) * | 2018-11-28 | 2019-05-03 | 昆明理工大学 | A kind of damaged tire cracking black carbon deliming and the method for ZnO recycling |
| CN110878148A (en) * | 2019-11-19 | 2020-03-13 | 珠海格力绿色再生资源有限公司 | Method for modifying pyrolysis carbon black |
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| CN113694891A (en) * | 2021-08-26 | 2021-11-26 | 华侨大学 | Method for preparing carbon black adsorbing material based on 3D printing |
| CN113694891B (en) * | 2021-08-26 | 2023-09-01 | 华侨大学 | Method for preparing carbon black adsorption material based on 3D printing |
| CN115446096A (en) * | 2022-08-29 | 2022-12-09 | 北京科技大学 | Method for preparing blast furnace injection fuel and zinc carbonate by cracking waste tire carbon black |
| CN115446096B (en) * | 2022-08-29 | 2023-08-08 | 北京科技大学 | Method for preparing blast furnace injection fuel and zinc carbonate by cracking carbon black from waste tires |
| GB2622610A (en) * | 2022-09-22 | 2024-03-27 | Ppp Portglenone Ltd | A method for obtaining carbon black, the carbon black obtained therefrom and the use thereof |
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| TW201813923A (en) | 2018-04-16 |
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