CN106433227A - Method for disposal and recycling of organic dead catalyst - Google Patents

Method for disposal and recycling of organic dead catalyst Download PDF

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Publication number
CN106433227A
CN106433227A CN201610792396.7A CN201610792396A CN106433227A CN 106433227 A CN106433227 A CN 106433227A CN 201610792396 A CN201610792396 A CN 201610792396A CN 106433227 A CN106433227 A CN 106433227A
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organic waste
waste catalyst
organic
rotary furnace
filter residue
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CN106433227B (en
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段琦
王瑞英
孔令超
孟翔
王通
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SHANDONG HUAAN NEW MATERIAL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00Liquid carbonaceous fuels
    • C10L1/32Liquid carbonaceous fuels consisting of coal-oil suspensions or aqueous emulsions or oil emulsions
    • C10L1/326Coal-water suspensions
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a method for disposal and recycling of an organic dead catalyst. The method comprises the first step of pressing the organic dead catalyst into an atomizer through nitrogen pressure to conduct atomizing, and sending the organic dead catalyst into a rotary furnace to conduct incineration, wherein atomizing pressure is 0.1-0.5 MPa, incineration temperature is 500-900 DEG C, and incineration temperature period is 60 s; the second step of conveying the product obtained in the first step to a reaction still after the product obtained in the first step cools down, adding water and stirring the product for 30-40 minutes, conducting filtration, conducting washing and filtration for three times after residues are neutralized by liquid sodium hydroxide to obtain washing water and residues; the third step of conducting grinding on the residues obtained in the second step, and making the grinded residues pass through a 325-mesh screen, wherein the sieving rate is 99.9% and the fourth step of conducting prilling, desiccation, sieving, magnetic separation and packaging on the product obtained in the third step to obtain a finished product carbon black. The method for disposal and recycling of the organic dead catalyst, on one hand, realizes innocent treatment on the organic dead catalyst, on the other hand turns dangerous solid waste into available products, thus solving the problem of environmental pollution and producing benefits at the same time.

Description

The process of a kind of organic waste catalyst and reuse method
Technical field
The present invention relates to process and the reuse method of a kind of organic waste catalyst, be specifically related to a kind of for organic reaction Useless positive acids, sulphonic acids, the process of the organic catalyst such as non-metal kind and reuse method.
Background technology
Organic reaction has very important status as the basis of chemical engineering industry in modern industry, entering of organic reaction Row tends not to individually carry out, and needs to introduce the third medium, i.e. catalyst in course of reaction.In numerous organic reaction processes In, the application of the organic catalysts such as positive acids, sulphonic acids, non-metal kind is relatively broad.With the carrying out of reaction, the work of catalyst Property be gradually lowered, when use some cycles after or because of misoperation cause catalyst to inactivate in advance, the activity of catalyst is not enough to When meeting the needs of reaction, mainly show as the conversion ratio decline of raw material, the selectivity decline of purpose product, accessory substance increase Several aspects, now need to carry out regenerating or changing to catalyst.For being processed into of the decaying catalyst that cannot be carried out regeneration The a great problem facing for current most chemical enterprise.Dead catalyst after inactivation be mainly composed of raw catalyst, Organic Ingredients, Sour gas etc..
It is to carry out high-temperature process by rotary furnace currently for the conventional processing method of this type of organic waste catalyst, make residual The material and supplies staying at high temperature reclaims, and uses the acidity easily having residual in the catalyst waste slag after this PROCESS FOR TREATMENT Gas, not only penetrating odor is relatively big, and has certain corrosivity, still falls within dangerous solid waste, has environment extremely strong Contaminative.
Content of the invention
The present invention, in order to make up the deficiencies in the prior art, provides process and the recycling side of a kind of organic waste catalyst Method, solution is widely used in process and the recycling of the organic catalysts such as the useless positive acids of organic reaction, sulphonic acids, non-metal kind Problem, the problem still falling within the dead catalyst of solid danger refuse after solving conventional treatment, solve the work that decaying catalyst is processed Skill problem and the pollution problem to environment.
The present invention is achieved through the following technical solutions:
The process of a kind of organic waste catalyst and reuse method, step is as follows:
(1) organic waste catalyst is pressed in atomizer by nitrogen pressurization, and spraying enters rotary furnace and burns, and burns generation Acid gas washes Systemic absorption, neutralization through scale;After nitrogen pressurization, control atomisation pressure is 0.1-0.5MPa, temperature when rotary furnace burns 500-900 DEG C, burn 60s;
(2) cooling down step (1) products therefrom, being delivered in reactor, add water washing, after stirring 30-40 minute, and mistake Filter, filter residue through in liquid caustic soda and after, then washing filtering three times, filter, obtain washings and filter residue, washings can be used for relieving haperacidity, filter residue Can be directly used as making the raw material of water-coal-slurry;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom carried out granulating, be dried, screen, magnetic separation, packaging, prepare finished product carbon black, for again Utilize.
Step (1) is burned the acid gas producing and is washed Systemic absorption, neutralization through scale.
Preferably, after the pressurization of step (1) nitrogen, control atomisation pressure is 0.2-0.4MPa, temperature 600-when rotary furnace burns 800℃.
Preferably, the fuel using in step (1) rotary furnace is natural gas, coal gas, the one in biogas.
Preferably, step (2) gained washings are used for relieving haperacidity, and filter residue is used as to make the raw material of water-coal-slurry.
Preferably, the comminutor using during step (4) granulation is wet granulator, a kind of type in squeezing comminutor.
Beneficial effects of the present invention:
The process of the present invention a kind of organic waste catalyst and reuse method solve conventional dead catalyst and process in technique The recycling problem of product carbon, in the method, organic waste catalyst harmful substance after burning all absorbs, it is not easy to have residual Sour gas, available part directly prepares water-coal-slurry or carbon black finished product, the whole process closed process of whole technical process, anacidity Property gas effusion.On the one hand achieving the harmless treatment to organic waste catalyst, being on the other hand changed into danger solid waste can The product utilizing, while bringing benefits, the problem that solves environmental pollution, economic benefit and social benefit are notable.
Detailed description of the invention
The process of 1 one kinds of organic waste catalyst of embodiment and reuse method, step is as follows:
(1) organic waste catalyst is by nitrogen pressurization press-in atomizer, and spraying enters the rotary furnace (fuel in rotary furnace For natural gas) burn, burn the acid gas producing and wash Systemic absorption, neutralization through scale;After nitrogen pressurization, control atomisation pressure is 0.1MPa, temperature 500 DEG C when rotary furnace burns, burn 60s;
(2) cooling down step (1) products therefrom, being delivered in reactor, add water washing, after stirring 30 minutes, filters, filter Slag through in liquid caustic soda and after, then washing filtering three times, filter, obtain washings and filter residue, washings are used for relieving haperacidity, and filter residue is directly used as Make the raw material of water-coal-slurry;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom is carried out granulating (during granulation, using wet granulator), drying, screening, magnetic separation, bag Dress, prepares finished product carbon black, for reusing.
The process of 2 one kinds of organic waste catalyst of embodiment and reuse method, step is as follows:
(1) organic waste catalyst is by nitrogen pressurization press-in atomizer, and spraying enters the rotary furnace (fuel in rotary furnace For coal gas) burn, burn the acid gas producing and wash Systemic absorption, neutralization through scale;After nitrogen pressurization, control atomisation pressure is 0.5MPa, temperature 900 DEG C when rotary furnace burns, burn 60s;
(2) cooling down step (1) products therefrom, being delivered in reactor, add water washing, after stirring 40 minutes, filters, filter Slag through in liquid caustic soda and after, then washing filtering three times, filter, obtain washings and filter residue, washings are used for relieving haperacidity, and filter residue is directly used as Make the raw material of water-coal-slurry;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom is carried out granulating (during granulation, using squeezing comminutor), drying, screening, magnetic separation, bag Dress, prepares finished product carbon black, for reusing.
The process of 3 one kinds of organic waste catalyst of embodiment and reuse method, step is as follows:
(1) organic waste catalyst is by nitrogen pressurization press-in atomizer, and spraying enters the rotary furnace (fuel in rotary furnace For natural gas) burn, burn the acid gas producing and wash Systemic absorption, neutralization through scale;After nitrogen pressurization, control atomisation pressure is 0.2MPa, temperature 600 DEG C when rotary furnace burns, burn 60s;
(2) cooling down step (1) products therefrom, being delivered in reactor, add water washing, after stirring 33 minutes, filters, filter Slag through in liquid caustic soda and after, then washing filtering three times, filter, obtain washings and filter residue, washings are used for relieving haperacidity, and filter residue is directly used as Make the raw material of water-coal-slurry;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom is carried out granulating (during granulation, using wet granulator), drying, screening, magnetic separation, bag Dress, prepares finished product carbon black, for reusing.
The process of 4 one kinds of organic waste catalyst of embodiment and reuse method, step is as follows:
(1) organic waste catalyst is by nitrogen pressurization press-in atomizer, and spraying enters the rotary furnace (fuel in rotary furnace For coal gas) burn, burn the acid gas producing and wash Systemic absorption, neutralization through scale;After nitrogen pressurization, control atomisation pressure is 0.4MPa, temperature 800 DEG C when rotary furnace burns, burn 60s;
(2) cooling down step (1) products therefrom, being delivered in reactor, add water washing, after stirring 37 minutes, filters, filter Slag through in liquid caustic soda and after, then washing filtering three times, filter, obtain washings and filter residue, washings are used for relieving haperacidity, and filter residue is directly used as Make the raw material of water-coal-slurry;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom is carried out granulating (during granulation, using squeezing comminutor), drying, screening, magnetic separation, bag Dress, prepares finished product carbon black, for reusing.
The process of 5 one kinds of organic waste catalyst of embodiment and reuse method, step is as follows:
(1) organic waste catalyst is by nitrogen pressurization press-in atomizer, and spraying enters the rotary furnace (fuel in rotary furnace For natural gas) burn, burn the acid gas producing and wash Systemic absorption, neutralization through scale;After nitrogen pressurization, control atomisation pressure is 0.3MPa, temperature 700 DEG C when rotary furnace burns, burn 60s;
(2) cooling down step (1) products therefrom, being delivered in reactor, add water washing, after stirring 35 minutes, filters, filter Slag through in liquid caustic soda and after, then washing filtering three times, filter, obtain washings and filter residue, washings are used for relieving haperacidity, and filter residue is directly used as Make the raw material of water-coal-slurry;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom is carried out granulating (during granulation, using wet granulator), drying, screening, magnetic separation, bag Dress, prepares finished product carbon black, for reusing.
The process of 6 one kinds of organic waste catalyst of embodiment and reuse method, step is as follows:
(1) organic waste catalyst is by nitrogen pressurization press-in atomizer, and spraying enters the rotary furnace (fuel in rotary furnace For coal gas) burn, burn the acid gas producing and wash Systemic absorption, neutralization through scale;After nitrogen pressurization, control atomisation pressure is 0.3MPa, temperature 700 DEG C when rotary furnace burns, burn 60s;
(2) cooling down step (1) products therefrom, being delivered in reactor, add water washing, after stirring 35 minutes, filters, filter Slag through in liquid caustic soda and after, then washing filtering three times, filter, obtain washings and filter residue, washings are used for relieving haperacidity, and filter residue is directly used as Make the raw material of water-coal-slurry;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom is carried out granulating (during granulation, using squeezing comminutor), drying, screening, magnetic separation, bag Dress, prepares finished product carbon black, for reusing.
Test example:The effect of process and reuse method in order to verify the present invention a kind of organic waste catalyst, the present invention People has done contrast test, is specifically divided into control group and experimental group.
Collect used organic waste catalyst in 3 kinds of chemical laboratories, be respectively the useless positive acids for organic reaction Organic catalyst, useless sulphonic acids organic catalyst, useless non-metal kind organic catalyst, respectively collect 30g.Useless by collect at random Positive acids organic catalyst, useless sulphonic acids organic catalyst, useless non-metal kind organic catalyst are divided evenly into three parts, every portion It point is 10g, numbered positive acids A, positive acids B, positive acids C, sulphonic acids A, sulphonic acids B, sulphonic acids C, non-metal kind A, non- Metal class B, non-metal kind C, all seal and place.
Wherein, positive acids A, sulphonic acids A, non-metal kind A are used for control group, use traditional treatment method, directly will respectively It burns, and measures the main component index of the product obtaining after burning, and concrete data are shown in Table 1.
Positive acids B, positive acids C, sulphonic acids B, sulphonic acids C, non-metal kind B, non-metal kind C are used for experimental group, adopt respectively Processing by the method for embodiment of the present invention 1-6, measuring the main component index of final products, concrete data are shown in Table 1.
Table 1:Main component index after different disposal for the different types of organic waste catalyst
From table 1, either to useless positive acids organic catalyst, or to useless sulphonic acids organic catalyst or the non-gold that gives up Belong to the process of class organic catalyst, use the iodine absorption value of the products therefrom after processing method of the present invention, CTAB adsorption specific surface area, 300% stress at definite elongation, oil factor are obviously higher than all index values of products therefrom after employing traditional treatment method;Meanwhile, adopt With the content of ashes and impurity content of the products therefrom after processing method of the present invention all significantly lower than employing traditional treatment method All index content of rear products therefrom.The performance of the processing method products therefrom of obvious organic waste catalyst of the present invention is more excellent Good, the grade quality of gained carbon black is higher, so the process of the present invention a kind of organic waste catalyst and reuse method are more excellent Useless ortho-acid, sulfonic acid, non-metallic organocatalyst process and recycling project.

Claims (6)

1. the process of organic waste catalyst and a reuse method, is characterized in that:Step is as follows:
(1) being pressed in atomizer by nitrogen pressurization by organic waste catalyst, spraying enters in rotary furnace, burns;Atomisation pressure For 0.1-0.5MPa, when rotary furnace burns, temperature is 500-900 DEG C, and the burning time is 60s;
(2) it after step (1) products therefrom being cooled down, is delivered in reactor, adds water, after stirring 30-40 minute, filter, filter residue Through in liquid caustic soda and after, then washing filtering three times, obtain washings and filter residue;
(3) step (2) gained filter residue is ground, cross 325 mesh sieves;Sieving rate is 99.9%;
(4) step (3) products therefrom carried out granulating, be dried, screen, magnetic separation, packaging, prepare finished product carbon black, for reusing.
2. the process of a kind of organic waste catalyst according to claim 1 and reuse method, is characterized in that:Step (1) Burn the acid gas producing and wash Systemic absorption, neutralization through scale.
3. the process of a kind of organic waste catalyst according to claim 1 and reuse method, is characterized in that:Step (1) After nitrogen pressurization, control atomisation pressure is 0.2-0.4MPa, temperature 600-800 DEG C when rotary furnace burns.
4. the process of a kind of organic waste catalyst according to claim 1 and reuse method, is characterized in that:Step (1) The fuel using in rotary furnace is natural gas, coal gas, the one in biogas.
5. the process of a kind of organic waste catalyst according to claim 1 and reuse method, is characterized in that:Step (2) Gained washings are used for relieving haperacidity, and filter residue is used as to make the raw material of water-coal-slurry.
6. the process of a kind of organic waste catalyst according to claim 1 and reuse method, is characterized in that:Step (4) The comminutor using during granulation is wet granulator, a kind of type in squeezing comminutor.
CN201610792396.7A 2016-08-31 2016-08-31 A kind of processing of organic dead catalyst and reuse method Active CN106433227B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112852513A (en) * 2021-01-12 2021-05-28 国家能源集团宁夏煤业有限责任公司 Coal water slurry, preparation method thereof and preparation method of synthesis gas

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102335668A (en) * 2010-07-19 2012-02-01 车磊 Method for treating industrial hazardous wastes containing organic solvent
CN204704822U (en) * 2015-06-19 2015-10-14 山东华安新材料有限公司 For the treatment system of the dead catalyst fluosulfonic acid that alkene or alkynes react

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102335668A (en) * 2010-07-19 2012-02-01 车磊 Method for treating industrial hazardous wastes containing organic solvent
CN204704822U (en) * 2015-06-19 2015-10-14 山东华安新材料有限公司 For the treatment system of the dead catalyst fluosulfonic acid that alkene or alkynes react

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CN112852513A (en) * 2021-01-12 2021-05-28 国家能源集团宁夏煤业有限责任公司 Coal water slurry, preparation method thereof and preparation method of synthesis gas

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Denomination of invention: A treatment and reuse method of organic waste catalyst

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