CN103540172B - Method and system for preparing regenerative carbon black by deashing and modifying pyrolytic carbon of waste rubber and plastic products - Google Patents
Method and system for preparing regenerative carbon black by deashing and modifying pyrolytic carbon of waste rubber and plastic products Download PDFInfo
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- CN103540172B CN103540172B CN201310534302.2A CN201310534302A CN103540172B CN 103540172 B CN103540172 B CN 103540172B CN 201310534302 A CN201310534302 A CN 201310534302A CN 103540172 B CN103540172 B CN 103540172B
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- 239000002296 pyrolytic carbon Substances 0.000 title claims abstract description 156
- 239000006229 carbon black Substances 0.000 title claims abstract description 48
- 239000004033 plastic Substances 0.000 title claims abstract description 48
- 229920003023 plastic Polymers 0.000 title claims abstract description 48
- 239000002699 waste material Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000001172 regenerating effect Effects 0.000 title abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 90
- 239000003513 alkali Substances 0.000 claims abstract description 38
- 150000003839 salts Chemical class 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 28
- 238000000197 pyrolysis Methods 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 11
- 230000008929 regeneration Effects 0.000 claims description 30
- 238000011069 regeneration method Methods 0.000 claims description 30
- 238000007599 discharging Methods 0.000 claims description 22
- 238000012986 modification Methods 0.000 claims description 20
- 230000004048 modification Effects 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 16
- 238000001556 precipitation Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000009434 installation Methods 0.000 claims description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 239000003610 charcoal Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005453 pelletization Methods 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000002737 fuel gas Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000012163 sequencing technique Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 4
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000003607 modifier Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 11
- 238000005336 cracking Methods 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 239000003738 black carbon Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 235000017550 sodium carbonate Nutrition 0.000 description 4
- 239000007822 coupling agent Substances 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000010920 waste tyre Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- -1 Titanic acid ester Chemical class 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processing Of Solid Wastes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method and a system for preparing regenerative carbon black by deashing and modifying pyrolytic carbon of waste rubber and plastic products. The method comprises the following steps: preparing the pyrolytic carbon from the waste rubber and plastic products through a pyrolytic process, and crushing the pyrolytic carbon; respectively carrying out two different acid reactions and one alkali reaction on the pyrolytic carbon to convert the vast majority of ash in the pyrolytic carbon into soluble salts; washing the pyrolytic carbon through water, and filtering to remove the soluble salts; reacting the deashed pyrolytic carbon with a modifier to change the micro chemical environment on the surface of the pyrolytic carbon to form a new combined layer and strength the binding force between the pyrolytic carbon particles and the rubber and the plastic so as to prepare the regenerative carbon black, and by means of the treatment, the ash content in the pyrolytic carbon is greatly decreased, and the waste rubber and plastic products are recycled. Meanwhile, the invention also discloses a system for preparing regenerative carbon black by deashing and modifying pyrolytic carbon of waste rubber and plastic products, and heat needed in the reaction process of the system is obtained from combustible gases generated by pyrolysis of the waste rubber and plastic products, so that cyclic utilization of energy source is realized.
Description
Technical field
The present invention relates to a kind of method and system of waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black, particularly a kind of method and system of the pyrolytic carbon ash disposal modification preparation, regeneration carbon black to pyrolytic carbon degree of depth ash disposal at high proportion, surface modification raising reinforcing effect.
Background technology
Along with the accelerated development of rubber, plastics industry, occur a large amount of waste rubber plastics in world wide, these rubber plastic products are usually containing high molecular polymer, carbon black and some ash contents.Containing elements such as zinc, calcium, silicon, aluminium, sodium, iron, magnesium, potassium, sulphur, phosphorus in ash content.
Along with technical progress, waste rubber converting-plastics can be charcoal, oil and inflammable gas by pyrolytic technique, but containing a large amount of ash content in pyrolytic carbon, ash content accounts for the 15%-20% of pyrolytic carbon mass ratio usually, this causes the performance of pyrolytic carbon and general industry carbon black, and there is a big difference, and particularly the existence of some ash content causes pyrolytic carbon to carry out recycle.
Application number be CN03129370.0, name is called in the Chinese patent of " a kind of production method of low ash content regenerative carbon cellulosic material ", disclose after under an inert atmosphere the charing of waste polymer material warms thermo-cracking being obtained cracking black carbon, add a kind of inorganic salt and this cracking black carbon is baking mixed, make inorganic salt be molten state and with the reactive metal oxide in this cracking black carbon, generate the metal-salt of solubility, through subsequent techniques such as washing, drying, crushing and classifications, prepare low ash content regenerative carbon cellulosic material.So this patent adopt inorganic salt and carbon black baking mixed, its dedusting effect is undesirable, and roasting required equipment is more complicated, expensive, and needed for roasting, the energy is more.
In addition, application number be CN201310165196.5, name is called in the Chinese patent of " a kind of solid phase graft-modification method regenerating cracking black carbon ", disclose in the pyrolytic carbon produced at waste old, plastics Pintsch process and add organic compound, by milling equipment, organifying compound situ-formed graft, to the surface of pyrolytic carbon, obtains the regeneration cracking black carbon of solid phase graft-modification.Organic compound is fully contacted with pyrolytic carbon surface, reacts by milling equipment by this patent, but its weak point is that this reaction effect is not good, and does not solve the high problem of pyrolytic carbon ash content.
Summary of the invention
The object of this invention is to provide a kind of can the method for waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black of suitability for industrialized production and device, use pyrolysis gas is the energy, the ash content in pyrolytic carbon is removed with better simply chemical reaction, change pyrolytic carbon surface micro-chemical environment, thus pyrolytic carbon is converted into the regeneration carbon black of similar general industry carbon black performance.
For achieving the above object, the present invention proposes following technical scheme: a kind of method of waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black, comprises the following steps:
Step one, waste rubber plastics obtain pyrolytic carbon by pyrolytic reaction;
Step 2, records various component proportions in ash oontent and ash content according to pyrolytic carbon, and described pyrolytic carbon and the first acid are fully reacted, part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; The first acid is selected from the combination of one or more in hydrochloric acid, sulfuric acid, hydrofluoric acid, phosphoric acid;
Step 3, records various component proportions in ash oontent and ash content according to pyrolytic carbon, and the pyrolytic carbon after step 2 process and the second acid are fully reacted, part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Described the second acid is selected from the combination of one or more in hydrochloric acid, sulfuric acid, hydrofluoric acid, phosphoric acid, and different from the composition of the first acid;
Step 4, is uniformly mixed the pyrolytic carbon after step 3 process and properties-correcting agent, heats while stirring to pyrolytic carbon, and described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, reacts under condition of normal pressure, and filtration after completing, obtains described regeneration carbon black; Described properties-correcting agent is selected from the combination of one or more in stearic acid, sodium stearate.
More preferably, between described step 2 and step 3, also comprise the reactions steps of pyrolytic carbon and alkali.
Described alkali is selected from the combination of one or more in sodium carbonate, sodium hydroxide, potassium hydroxide;
The reaction conditions of described pyrolytic carbon and alkali is temperature 70 C ~ 100 DEG C, normal pressure or temperature 120 DEG C ~ 151 DEG C, pressure 0.2MPa ~ 0.5MPa.
Reaction conditions in described step 2, step 3 is temperature 70 C ~ 100 DEG C, normal pressure or temperature 120 DEG C ~ 151 DEG C, pressure 0.2MPa ~ 0.5MPa.
The present invention also proposes a kind of technical scheme of system of waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black, comprises acid-respons container, modified-reaction container, sprinkling equipment, filter plant, precipitation and water treatment system; Wherein said acid-respons container is connected with modified-reaction container, is respectively used to pyrolytic carbon and acid and properties-correcting agent to react; Described sprinkling equipment is connected with acid-respons container, neutralizes for the gas produced acid-respons, absorbs; Described filter plant is arranged on the rear road of acid-respons container and modified-reaction container, carries out solid-liquid separation for the discharging after completing acid-respons, modified-reaction; Described precipitation and water treatment system are connected with described filter plant, for precipitating the solids filtered in rear gained filtrate.
More preferably, described system also comprises the alkali reaction container be connected with described acid-respons container and modified-reaction container, and described alkali reaction container is used for described pyrolytic carbon and alkali to react.
Described system also comprises the granulating equipment be connected with filter plant, and described granulating equipment is used for powdery to regenerate pelletizing of carbon black.
Described system also comprise shredder assembly, pyrolysis installation, shredding unit and gas fired-boiler; Waste rubber plastics are broken into particle by described shredder assembly; The pyrolysis of waste rubber plastics is become pyrolytic carbon, oil and combustible gas by described pyrolysis installation; Described shredding unit exports with the charcoal of pyrolysis installation and is connected, for being pulverized by pyrolytic carbon; Described gas fired-boiler is connected with the gas outlet of pyrolysis installation, for by pyrolysis fuel gas buring water vapour.
Ash conversion in pyrolytic carbon for raw material, is soluble salt by twice different acid-respons and alkali reaction with waste rubber plastics pyrolytic carbon by the present invention, then by washing, filter salt be separated from pyrolytic carbon, realize ash disposal; Change pyrolytic carbon surface micro-chemical environment by modified-reaction, form new key coat, enhances pyrolysis carbon granule and rubber, bonding force between plastics, improve reinforcing effect, thus obtained regeneration carbon black, substantially reach the performance index of general industry carbon black.
The reaction process of described pyrolytic carbon and the first acid comprises: add in pyrolytic carbon by the first acid, be uniformly mixed, while stirring, pyrolytic carbon is heated, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with the first acid under 0.2MPa ~ 0.5MPa condition, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Remaining pyrolytic carbon proceeds ensuing reaction.
The reaction process of described pyrolytic carbon and alkali comprises: added by alkali in pyrolytic carbon, be uniformly mixed, while stirring, pyrolytic carbon is heated, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with alkali under 0.2MPa ~ 0.5MPa condition, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Remaining pyrolytic carbon proceeds ensuing reaction.
The reaction process of described pyrolytic carbon and the second acid comprises: add in pyrolytic carbon by the second acid, be uniformly mixed, while stirring, pyrolytic carbon is heated, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with the second acid under 0.2MPa ~ 0.5MPa condition, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Remaining pyrolytic carbon proceeds ensuing reaction.
The reaction process of described pyrolytic carbon and properties-correcting agent comprises: added by properties-correcting agent in pyrolytic carbon, be uniformly mixed, heat while stirring to pyrolytic carbon, and described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, reacts under condition of normal pressure, filtration after completing.Obtained regeneration carbon black can be further processed.
Compared with prior art, ash oontent can be reduced to 1%-2% up to the ash oontent of the original pyrolytic carbon of 20% by the present invention, the reinforcement ability of obtained regeneration carbon black can compare favourably with the industrial carbon black such as N330, N660, realizes the recycle of waste rubber plastics.More meaningfully, in above-mentioned reaction, drying process, institute's heat requirement comes from the combustible gas that the pyrolysis of waste rubber plastics produces, and has both avoided the outer pollution discharging environment of pyrolysis gas, and has fully realized recycle again.
Accompanying drawing explanation
Fig. 1 is the schema of the method for waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black of the present invention;
Fig. 2 is the schema of Fig. 1 refinement;
Fig. 3 is the structural representation of the system of waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black of the present invention.
In figure, element numbers is:
Waste rubber plastic breaker 1, transfer roller 21 ~ 28, pyrolysis installation 3; pyrolytic carbon shredding unit 4, gas fired-boiler 5, sour A reaction vessel 6; filter plant 71 ~ 74, alkali B reaction vessel 8, alkali spray column 9; acid C reaction vessel 10; modified-reaction container 11, tablets press 12, drying plant 13; packaging facilities 14, precipitation and water treatment system 15
Embodiment
Below in conjunction with accompanying drawing of the present invention, clear, complete description is carried out to the technical scheme of the embodiment of the present invention.
Described in composition graphs 1, Fig. 2, the method for waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black of the present invention comprises the following steps:
S1, waste rubber plastics adopt pyrolytic process to obtain pyrolytic carbon, oil, combustible gas.
S2, pyrolytic carbon is crushed to the following fineness of 325 order (particle diameter < 45 μm).
S3, pyrolytic carbon and sour A react, and part of ash is changed into soluble salt, then remove through washing and filtering.
Specifically, the reaction process of pyrolytic carbon and sour A comprises: add in pyrolytic carbon by sour A, be uniformly mixed, while stirring, pyrolytic carbon is heated, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with sour A under the condition of 0.2MPa ~ 0.5MPa, and reaction rear section ash conversion becomes soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Remaining pyrolytic carbon proceeds subsequent reactions.Wherein sour A is selected from the combination of one or more in hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, phosphoric acid.
S4, pyrolytic carbon and alkali B react, and part of ash is changed into soluble salt, then remove through washing and filtering.
Specifically, the process that pyrolytic carbon and alkali B react comprises: add in pyrolytic carbon by alkali B, be uniformly mixed, while stirring, pyrolytic carbon is heated, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with alkali under 0.2MPa ~ 0.5MPa condition, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Remaining pyrolytic carbon proceeds subsequent reactions.Alkali B is the combination of one or more in sodium carbonate, sodium hydroxide, potassium hydroxide.
The step that pyrolytic carbon and alkali B react is optional step, and according to the ash content kind of waste rubber plastics is different, whether selection adopts.
S4, pyrolytic carbon and sour C react, and part of ash is changed into soluble salt, then remove through washing and filtering.
Specifically, the process that pyrolytic carbon and sour C react comprises: add in pyrolytic carbon by sour C, be uniformly mixed, while stirring, pyrolytic carbon is heated, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with sour C under 0.2MPa ~ 0.5MPa condition, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Remaining pyrolytic carbon proceeds subsequent reactions.Acid C is the combination of one or more in hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, phosphoric acid, and different from sour A composition.
For different waste rubber plastics pyrolytic carbons, interchangeable scheme is, the sequencing of S3, S4, S5 can change.
S6, pyrolytic carbon and properties-correcting agent D react, and change pyrolytic carbon surface micro-chemical environment, form new key coat, and enhances pyrolysis carbon granule and rubber, bonding force between plastics, improve reinforcing effect, thus obtained regeneration carbon black.
Specifically, the process that pyrolytic carbon and properties-correcting agent D react comprises: add in pyrolytic carbon by properties-correcting agent D, be uniformly mixed, heat while stirring to pyrolytic carbon, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, reacts under condition of normal pressure, filtration after completing.Obtained regeneration carbon black proceeds described step 7.Properties-correcting agent D is the combination of one or more in silane coupling agent, titanate coupling agent, aluminate coupling agent, stearic acid, sodium stearate.
S7, ash disposal modified gained regeneration carbon black is through granulation, drying, packaging, available.
As shown in Figure 3, the system of disclosed a kind of waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black, comprises waste rubber plastic breaker 1; transfer roller 21 ~ 27, pyrolysis installation 3, pyrolytic carbon shredding unit 4; gas fired-boiler 5, sour A reaction vessel 6, filter plant 71 ~ 74; alkali B reaction vessel 8, alkali spray column 9, sour C reaction vessel 10; modified-reaction container 11, tablets press 12, drying plant 13; packaging facilities 14, precipitation and water treatment system 15.Waste rubber plastic crushing to particle diameter 2-5cm particle, is entered described pyrolysis installation 3, as the raw material of pyrolytic reaction by described transfer roller 21 by described crusher 1.
Waste rubber plastics are changed into pyrolytic carbon, oil and combustible gas by pyrolysis installation 3.Combustible gas inputs to the burning of described gas fired-boiler 5 and produces steam for reaction vessel, drying plant.Pyrolytic carbon is crushed to the following fineness of 325 order (particle diameter < 45 μm) by described shredding unit 4, delivers to sour A reaction vessel 6 through described transfer roller 22.Pyrolytic carbon reacts with sour A in reaction vessel 6, and the part of ash in pyrolytic carbon is changed into soluble salt.The collection and confinement of gases produced in reaction process, to described alkali spray column 9, is arranged after treatment.After having reacted, reaction vessel 6 discharging is filtered by described filter plant 71, then is washed with water by filter residue, filters.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
The filter residue that filter plant 71 produces delivers to alkali B reaction vessel 8 through described transfer roller 23.Pyrolytic carbon reacts with alkali B in reaction vessel 8, and the part of ash in pyrolytic carbon is changed into soluble salt.After having reacted, reaction vessel 8 discharging is filtered by described filter plant 72, then is washed with water by filter residue, filters.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
The filter residue that filter plant 72 produces delivers to sour C reaction vessel 10 through described transfer roller 24.Pyrolytic carbon reacts with sour C in reaction vessel 10, and the part of ash in pyrolytic carbon is changed into soluble salt.The collection and confinement of gases produced in reaction process, to described alkali spray column 9, is arranged after treatment.After having reacted, reaction vessel 10 discharging is filtered by described filter plant 73, then is washed with water by filter residue, filters.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
Introduce the process of the acid of waste rubber plastics pyrolytic carbon, alkali ash disposal reaction in front, the postpone of alkali B reaction vessel 8 placed in the middle, sour C reaction vessel 10 with sour A reaction vessel 6 in the present embodiment, in other embodiments, described sour A reaction vessel 6, alkali B reaction vessel 8, sour C reaction vessel 10 connect front and back position can specifically contained by waste rubber plastics pyrolytic carbon the difference of ash content kind carry out front and back replacing, some embodiment also can omit alkali B reaction vessel 8.
The filter residue that filter plant 73 produces delivers to modified-reaction container 11 through described transfer roller 25.Pyrolytic carbon reacts with properties-correcting agent D in reaction vessel 11, obtained regeneration carbon black.Reaction vessel 11 discharging is filtered by described filter plant 74.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
Obtained regeneration carbon black delivers to tablets press 12 through described transfer roller 26, will regenerate pelletizing of carbon black.Carbon black particle delivers to drying plant 13 through described transfer roller 27, carries out drying.Dried carbon black particle is delivered to packaging facilities 14 through described transfer roller 28 and is packed.
Below for waste tyre pyrolytic charcoal ash disposal modification preparation, regeneration carbon black, the process of the present invention to waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black is described.Damaged tire delivers to crusher 1 by e Foerderanlage (not shown), is broken into the micelle of 2-5cm.Micelle enters pyrolysis installation 3 by transfer roller 21, changes into pyrolytic carbon, oil and combustible gas through pyrolytic reaction.Combustible gas inputs to the burning of described gas fired-boiler 5 and produces steam for reaction vessel, drying plant.Pyrolytic carbon is crushed to 325 orders by shredding unit 4, delivers to sour A reaction vessel 6 through transfer roller 22.Pyrolytic carbon reacts with hydrochloric acid (sour A) in reaction vessel 6, and the part of ash in pyrolytic carbon is changed into soluble salt.The collection and confinement of gases produced in reaction process, to alkali spray column 9, is arranged after treatment.After having reacted, reaction vessel 6 discharging is filtered by filter plant 71, then is washed with water by filter residue, filters.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
The filter residue that filter plant 71 produces delivers to alkali B reaction vessel 8 through transfer roller 23.Pyrolytic carbon reacts with soda ash (alkali B) in reaction vessel 8, and the part of ash in pyrolytic carbon is changed into soluble salt.After having reacted, reaction vessel 8 discharging is filtered by filter plant 72, then is washed with water by filter residue, filters.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
The filter residue that filter plant 72 produces delivers to sour C reaction vessel 10 through described transfer roller 24.Pyrolytic carbon reacts with nitric acid (sour C) in reaction vessel 10, and the part of ash in pyrolytic carbon is changed into soluble salt.The collection and confinement of gases produced in reaction process, to alkali spray column 9, is arranged after treatment.After having reacted, reaction vessel 10 discharging is filtered by filter plant 73, then is washed with water by filter residue, filters.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
Above-mentioned hydrochloric acid, nitric acid, soda ash add-on record various component proportions in ash oontent and ash content according to pyrolytic carbon and determine.
The filter residue that filter plant 73 produces delivers to modified-reaction container 11 through transfer roller 25.Pyrolytic carbon reacts with titanate coupling agent CT-136 in reaction vessel 11, obtained regeneration carbon black.Titanic acid ester add-on is the 1%-2% of pyrolytic carbon quality.Reaction vessel 11 discharging is filtered by described filter plant 74.Filtrate collection, to precipitation and water treatment system 15, is arranged outside after treated environment protection standard.
Obtained regeneration carbon black delivers to tablets press 12 through transfer roller 26, will regenerate pelletizing of carbon black.Carbon black particle delivers to drying plant 13 through transfer roller 27, carries out drying.Dried carbon black particle is delivered to packaging facilities 14 through transfer roller 28 and is packed.
After above-mentioned process, the ash oontent of waste tyre pyrolytic charcoal is reduced to 1.5%, DBP adsorptive value 85, tensile strength 17MPa from 18%, tensile yield 440%, 300% stress at definite elongation 8.1MPa.Performance index and general industry carbon black N330, N660 close.
Technology contents of the present invention and technical characteristic have disclosed as above; but those of ordinary skill in the art still may do all replacement and the modification that do not deviate from spirit of the present invention based on teaching of the present invention and announcement; therefore; scope should be not limited to the content that embodiment discloses; and various do not deviate from replacement of the present invention and modification should be comprised, and contained by present patent application claim.
Claims (6)
1. a method for waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black, is characterized in that comprising the following steps:
Step one, waste rubber plastics obtain pyrolytic carbon by pyrolytic reaction;
Step 2, various component proportions in ash oontent and ash content is recorded according to pyrolytic carbon, described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with the first acid under the condition of 0.2MPa ~ 0.5MPa, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; The first acid is selected from the combination of one or more in hydrochloric acid, sulfuric acid, hydrofluoric acid, phosphoric acid;
Step 3, various component proportions in ash oontent and ash content is recorded according to pyrolytic carbon, pyrolytic carbon after step 2 process is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with alkali under the condition of 0.2MPa ~ 0.5MPa, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Alkali is the combination of one or more in sodium carbonate, sodium hydroxide, potassium hydroxide;
Step 4, various component proportions in ash oontent and ash content is recorded according to pyrolytic carbon, pyrolytic carbon after step 3 process is 70 DEG C ~ 100 DEG C in temperature, under condition of normal pressure or in temperature is 120 DEG C ~ 151 DEG C, pressure is fully react with the second acid under the condition of 0.2MPa ~ 0.5MPa, and part of ash changes into soluble salt; Wash pyrolytic carbon, discharging filtering after having reacted with water, remove soluble salt; Described the second acid is selected from the combination of one or more in hydrochloric acid, sulfuric acid, hydrofluoric acid, phosphoric acid, and different from the composition of the first acid;
Step 5, is uniformly mixed the pyrolytic carbon after step 4 process and properties-correcting agent, heats while stirring to pyrolytic carbon, and described pyrolytic carbon is 70 DEG C ~ 100 DEG C in temperature, reacts under condition of normal pressure, and filtration after completing, obtains described regeneration carbon black; Described properties-correcting agent is selected from the combination of one or more in stearic acid, sodium stearate.
2. method according to claim 1, is characterized in that, the step of described step 3 pyrolytic carbon and alkali reaction is optional step, and according to the ash content kind of waste rubber plastics is different, whether selection adopts.
3. method according to claim 1, is characterized in that, for different waste rubber plastics pyrolytic carbons, interchangeable scheme is, the sequencing of step 2, step 3, step 4 can change.
4. a system for waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black, is characterized in that, comprises acid-respons container, alkali reaction container, modified-reaction container, sprinkling equipment, filter plant, precipitation and water treatment system; Wherein said acid-respons container is connected with modified-reaction container, is respectively used to pyrolytic carbon and acid and properties-correcting agent to react; Described alkali reaction container is connected with described acid-respons container and modified-reaction container, for described pyrolytic carbon and alkali being reacted; Described sprinkling equipment is connected with acid-respons container, neutralizes for the gas produced acid-respons, absorbs; Described filter plant is arranged on the rear road of acid-respons container and modified-reaction container, carries out solid-liquid separation for the discharging after completing acid-respons, modified-reaction; Described precipitation and water treatment system are connected with described filter plant, for precipitating the solids filtered in rear gained filtrate.
5. the system of waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black according to claim 4, is characterized in that, also comprise the granulating equipment be connected with filter plant, and described granulating equipment is used for powdery to regenerate pelletizing of carbon black.
6. the system of waste rubber plastics pyrolytic carbon ash disposal modification preparation, regeneration carbon black according to claim 4, is characterized in that, also comprise shredder assembly, pyrolysis installation, shredding unit and gas fired-boiler; Waste rubber plastics are broken into particle by described shredder assembly; The pyrolysis of waste rubber plastics is become pyrolytic carbon, oil and combustible gas by described pyrolysis installation; Described shredding unit exports with the charcoal of pyrolysis installation and is connected, for being pulverized by pyrolytic carbon; Described gas fired-boiler is connected with the gas outlet of pyrolysis installation, for by pyrolysis fuel gas buring water vapour.
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| PL240458B1 (en) * | 2018-04-17 | 2022-04-04 | Syntoil Spolka Akcyjna | Method for purification of carbonizate |
| CN109705635B (en) * | 2018-11-28 | 2021-02-26 | 昆明理工大学 | Method for deashing and recycling ZnO of waste tire pyrolysis carbon black |
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| CN111484649A (en) * | 2020-03-30 | 2020-08-04 | 青岛黑猫新材料研究院有限公司 | Preparation method of modified thermal cracking carbon black |
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| CN112246823A (en) * | 2020-09-08 | 2021-01-22 | 新奥生物质能(天津)有限公司 | High ash pyrolytic carbon utilization method and system |
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| CN114045523B (en) * | 2021-12-02 | 2023-07-28 | 郑州轻工业大学 | Waste tire pyrolytic carbon catalyst, preparation method and application |
| CN114381290A (en) * | 2022-02-12 | 2022-04-22 | 安徽固瑞特新材料科技有限公司 | Method for preparing superfine waste tire thermal cracking carbon black for rubber by wet method |
| CN114634722A (en) * | 2022-04-06 | 2022-06-17 | 安徽固瑞特新材料科技有限公司 | Method for improving structure of regenerated 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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Denomination of invention: Method and system for preparation of regenerated carbon black by removing ash from pyrolytic carbon of waste rubber plastic products Effective date of registration: 20210629 Granted publication date: 20150701 Pledgee: Bank of China Limited Suzhou Wuzhong sub branch Pledgor: Lianzhi Tongda (Suzhou) Environmental Technology Co.,Ltd. Registration number: Y2021320010226 |
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