CN109320112A - Utilize the high-intensitive geo-polymer and preparation method of the preparation of FCC dead catalyst - Google Patents

Utilize the high-intensitive geo-polymer and preparation method of the preparation of FCC dead catalyst Download PDF

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Publication number
CN109320112A
CN109320112A CN201711133468.8A CN201711133468A CN109320112A CN 109320112 A CN109320112 A CN 109320112A CN 201711133468 A CN201711133468 A CN 201711133468A CN 109320112 A CN109320112 A CN 109320112A
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China
Prior art keywords
polymer
geo
dead catalyst
fcc dead
preparation
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CN201711133468.8A
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Chinese (zh)
Inventor
张志远
张宏哲
房师平
牟桂芹
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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Priority to CN201711133468.8A priority Critical patent/CN109320112A/en
Publication of CN109320112A publication Critical patent/CN109320112A/en
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
    • C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/24—Cements from oil shales, residues or waste other than slag
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a kind of high-intensitive geo-polymers and preparation method using the preparation of FCC dead catalyst, are related to the preparation technical field of geo-polymer.This method will be added thereto exciting agent and stir evenly, will stir evenly gained mixture and pour into die for molding and ram-jolt after the grinding of FCC dead catalyst, and finally maintenance and is demoulded to age up to geo-polymer under certain curing condition.The present invention is using FCC dead catalyst as raw material, it is added with the activity of waterglass exciting agent excitation FCC dead catalyst as main component, the geo-polymer inorganic material of formation, high-intensitive geo-polymer is formed by maintenance afterwards, building materials are formed, have many advantages, such as that simple, at low cost, the innoxious effect of process flow is good.

Description

Utilize the high-intensitive geo-polymer and preparation method of the preparation of FCC dead catalyst
Technical field
The present invention relates to the preparation technical fields of geo-polymer, and in particular to it is a kind of using FCC dead catalyst preparation Geo-polymer and preparation method.
Background technique
So that catalyst activity is accelerated decline by heavy metal pollution due to catalyst in catalytic cracking unit, leads to catalyst Reaction selectivity be deteriorated, if only running damage by nature and to supplement new agent be the activity and selectivity for being unable to maintain that poising agent, Therefore need periodically to draw off a part of poising agent to guarantee that the activity and selectivity of catalyst in device is horizontal.It is this draw off it is flat Weighing apparatus agent is known as catalytic cracking spent catalyst (hereinafter referred to as dead catalyst).Dead catalyst activity is low, and contains an a certain amount of huge sum of money Belong to, pollution is strong, and harmless treatment is difficult, and the random processing for not conforming to specification can constitute a serious threat to environment for human survival.
Many research institutions start with certain ingredients in dead catalyst and are recycled as raw material both at home and abroad, this Environmental pollution is not only reduced, and reduces product cost.Patent CN201510194951.1 proposes a kind of catalytic cracking The method that dead catalyst recycles, this method are being supplemented using catalytic cracking spent catalyst, roasting kaolin microballoon as primary raw material Silicon source in the case where not adding additional silicon source, prepares fresh catalyst Cracking catalyst by the method for in-situ crystallization to make to urge Change cracking dead catalyst to be reused.The method that catalytic cracking spent catalyst provided by the invention recycles is split with existing catalysis Change the method that dead catalyst recycles to compare, method is simple, and low energy consumption, and prepared fresh catalyst Cracking catalyst is able to carry out Industrial application.Patent CN201610489957.6 proposes a kind of method of recovering rare earth from catalytic cracking spent catalyst, this Method is that the catalytic cracking spent catalyst containing rare earth is placed in in the sulfuric acid solution of the 20%-65% at 100-150 DEG C acid is molten, Addition ammonium hydroxide in solution is stated then up and obtains rare-earth enrichment liquid, will be obtained after moisture evaporation in pregnant solution using the method for evaporation Sulfuric acid rare earth double salt product.This kind of method is easy to operate, at low cost, and rare earth yield is high, is a kind of energy-efficient rare earth time Receiving method.
Method disclosed in the above-mentioned prior art all thinks rare earth, heavy metal and molecular sieve on FCC dead catalyst It is all valuable substance, consideration is all how to be recycled.Moreover, there are the weights such as Ni, V, Sb in FCC dead catalyst Metal is a kind of danger wastes.Its main component is SiO2、Al2O3Equal sieve and silica-sesquioxides and metal oxide, meet geology The component requirements condition of polymer, and by 700 DEG C of roasting, reactivity with higher.But it is at present making During geo-polymer, the problems such as maintenance of simple room temperature will appear crackle, and later strength is not high.
Summary of the invention
The purpose of the present invention is to provide a kind of high-intensitive geo-polymer using the preparation of FCC dead catalyst and preparation sides Method is to conserve parameter using FCC dead catalyst as raw material to molding geo-polymer by regulation, improve synthesized geology The intensity of polymer, the method for the present invention also achieve the resource to FCC dead catalyst while improving geo-polymer intensity Change and utilizes.
One of task of the invention is to provide a kind of method for preparing geo-polymer using FCC dead catalyst, successively The following steps are included:
After a grinds the FCC dead catalyst, exciting agent is added thereto and stirs evenly；
Step a is stirred evenly gained mixture and pours into die for molding and ram-jolt by b；
C is conserved under certain curing condition to age, and is demoulded up to geo-polymer.
Direct advantageous effects brought by above-mentioned technical proposal are:
Heavy metal in FCC dead catalyst is subjected to solidification harmlessness disposing, obtained geo-polymer heavy metal is no longer It leaches, no longer endangers environment, be equivalent to and solve the environmentally hazardous basic problem of hazardous waste.
By the way that exciting agent is added into FCC dead catalyst, and by regulation maintenance parameter, it is poly- to obtain high-intensitive geology Object is closed, further demonstrating above-mentioned conclusion by following embodiments is to set up.
As a preferred solution of the present invention, the partial size after the FCC dead catalyst grinding is 100 mesh.
As another preferred embodiment of the invention, the exciting agent is sodium silicate solution, the sodium silicate solution Modulus control is 1.5.
Preferably, sodium hydroxide and calcium oxide are added into step a.
Further, it is stirred evenly in step a in the net paddle stirring machine total mix merging of cement.
Further, 5~15min is shaken in step b in vibration analyzer.
Further, the curing condition are as follows: 25 DEG C~85 DEG C of temperature, humidity 50%~95% conserve 10 days.
The two of task of the invention are to provide the geo-polymer that the above method is prepared, the geo-polymer Compression strength is 14.2MPa~29.4MPa.
Another task of the invention is to provide application of the above-mentioned geo-polymer in materials for wall.
The present invention is realized rationally sharp to the recycling of FCC dead catalyst by selecting FCC dead catalyst as raw material With by the way that exciting agent is added into FCC dead catalyst, by regulation to molding geo-polymer maintenance parameter, raising is closed At the intensity of geo-polymer, high-intensitive building materials are formed, in case the utilization of resources.
Specific embodiment
The invention discloses it is a kind of using FCC dead catalyst preparation high-intensitive geo-polymer and preparation method, in order to Keep advantages of the present invention, technical solution clearer, clear, elaborates combined with specific embodiments below to the present invention.
Primary raw material selected by the present invention is done as described below:
FCC dead catalyst partial size should be in 100 mesh.
Exciting agent is preferably sodium silicate aqueous solution, modulus 1.5.
Embodiment 1:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition is 25 DEG C, 50% conserves 10 days.It obtains The Leaching of geo-polymer nickel element drops to 0.09ppm by 2.85ppm；Compression strength is 14.2MPa.
Embodiment 2:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition is 25 DEG C of room temperature, 75% maintenance 10 days.? To the Leaching of geo-polymer nickel element 0.09ppm is dropped to by 2.85ppm；Compression strength is 18.1MPa.
Embodiment 3:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition is 25 DEG C, 95% conserves 10 days.It obtains The Leaching of geo-polymer nickel element drops to 0.09ppm by 2.85ppm；Compression strength is 19.3MPa.
Embodiment 4:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition is 55 DEG C, 50% conserves 10 days.It obtains The Leaching of geo-polymer nickel element drops to 0.09ppm by 2.85ppm；Compression strength is 28.7MPa.
Embodiment 5:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition be 55 DEG C 75% thermostatic curing 10 days.? To the Leaching of geo-polymer nickel element 0.09ppm is dropped to by 2.85ppm；Compression strength is 29.4MPa.
Embodiment 6:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition is 55 DEG C 95% of constant humidity and conserves 10 days.? To the Leaching of geo-polymer nickel element 0.09ppm is dropped to by 2.85ppm；Compression strength is 26.3MPa.
Embodiment 7:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition is 85 DEG C, 50% conserves 10 days.It obtains The Leaching of geo-polymer nickel element drops to 0.09ppm by 2.85ppm；Compression strength is 24.3MPa.
Embodiment 8:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition be 85 DEG C 75% thermostatic curing 10 days.? To the Leaching of geo-polymer nickel element 0.09ppm is dropped to by 2.85ppm；Compression strength is 22.1MPa.
Embodiment 9:
The experiment of 300g dead catalyst, experiment condition: the waterglass that modulus is 1.5 is added in 100 mesh of partial size；Speed of agitator: from Turn 300/min, revolve 110/min；Molding die: 40*40*160mm；Curing condition is 85 DEG C 95% of constant humidity and conserves 10 days.? To the Leaching of geo-polymer nickel element 0.09ppm is dropped to by 2.85ppm；Compression strength is 20.3MPa.
It should be noted that any equivalent way that those skilled in the art are made under the introduction of this specification, or Obvious variant should all be within the scope of the present invention.

Claims (9)

1. a kind of method for preparing geo-polymer using FCC dead catalyst, which is characterized in that successively the following steps are included:
After a grinds the FCC dead catalyst, exciting agent is added thereto and stirs evenly；
Step a is stirred evenly gained mixture and pours into die for molding and ram-jolt by b；
C is conserved under certain curing condition to age, and is demoulded up to geo-polymer.
2. the method according to claim 1 for preparing geo-polymer using FCC dead catalyst, it is characterised in that: described Partial size after the grinding of FCC dead catalyst is 100 mesh.
3. the method according to claim 1 for preparing geo-polymer using FCC dead catalyst, it is characterised in that: described Exciting agent be sodium silicate solution, the sodium silicate solution modulus control be 1.5.
4. the method according to claim 1 for preparing geo-polymer using FCC dead catalyst, it is characterised in that: Xiang Bu Sodium hydroxide and calcium oxide is added in rapid a.
5. the method according to claim 1 for preparing geo-polymer using FCC dead catalyst, it is characterised in that: step a In stirred evenly in cement net paddle stirring machine total mix merging.
6. the method according to claim 1 for preparing geo-polymer using FCC dead catalyst, it is characterised in that: step b In in vibration analyzer shake 5~15min.
7. the method according to claim 1 for preparing geo-polymer using FCC dead catalyst, it is characterised in that: described Curing condition are as follows: 25 DEG C~85 DEG C of temperature, humidity 50%~95% conserve 10 days.
8. the geo-polymer that described in any item methods are prepared according to claim 1~7, it is characterised in that: describedly The compression strength of matter polymer is 14.2MPa~29.4MPa.
9. application of the geo-polymer according to claim 8 in materials for wall.
CN201711133468.8A 2017-11-16 2017-11-16 Utilize the high-intensitive geo-polymer and preparation method of the preparation of FCC dead catalyst Pending CN109320112A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110255936A (en) * 2019-06-28 2019-09-20 武汉科技大学 A method of strengthening metakaolin based geopolymer performance
CN110540435A (en) * 2019-09-25 2019-12-06 山东京博环保材料有限公司 autoclaved aerated concrete prepared by utilizing waste FCC catalyst and preparation method thereof
CN111847934A (en) * 2019-04-26 2020-10-30 中国石油化工股份有限公司 Soil-polymerized cement material and its preparing process
CN112573863A (en) * 2019-09-29 2021-03-30 中国石油化工股份有限公司 Preparation method for improving intensity of geopolymer of catalytic cracking waste catalyst
CN114572994A (en) * 2022-02-28 2022-06-03 西藏大学 Zeolite-like material and preparation method and application thereof

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US20110039687A1 (en) * 2009-08-17 2011-02-17 Epel Co., Ltd. Catalyst for recovering light oil and preparation method thereof
CN102633449A (en) * 2012-05-03 2012-08-15 南京大学 High-strength glass base polymer and preparation method thereof
CN104098281A (en) * 2013-04-03 2014-10-15 神华集团有限责任公司 Geopolymer composition, geopolymer material and preparation method thereof
CN105693120A (en) * 2016-01-31 2016-06-22 西安建筑科技大学 Preparation and application of conductivity-controllable fly ash-based geopolymer material
CN106140296A (en) * 2015-04-22 2016-11-23 中国石油化工股份有限公司 A kind of method of catalytic cracking spent catalyst recycling

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Publication number Priority date Publication date Assignee Title
CN101492276A (en) * 2009-02-19 2009-07-29 广西大学 Novel clay soil polyporous materials and method of producing the same
US20110039687A1 (en) * 2009-08-17 2011-02-17 Epel Co., Ltd. Catalyst for recovering light oil and preparation method thereof
CN102633449A (en) * 2012-05-03 2012-08-15 南京大学 High-strength glass base polymer and preparation method thereof
CN104098281A (en) * 2013-04-03 2014-10-15 神华集团有限责任公司 Geopolymer composition, geopolymer material and preparation method thereof
CN106140296A (en) * 2015-04-22 2016-11-23 中国石油化工股份有限公司 A kind of method of catalytic cracking spent catalyst recycling
CN105693120A (en) * 2016-01-31 2016-06-22 西安建筑科技大学 Preparation and application of conductivity-controllable fly ash-based geopolymer material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111847934A (en) * 2019-04-26 2020-10-30 中国石油化工股份有限公司 Soil-polymerized cement material and its preparing process
CN111847934B (en) * 2019-04-26 2022-07-12 中国石油化工股份有限公司 Soil-polymerized cement material and its preparing process
CN110255936A (en) * 2019-06-28 2019-09-20 武汉科技大学 A method of strengthening metakaolin based geopolymer performance
CN110540435A (en) * 2019-09-25 2019-12-06 山东京博环保材料有限公司 autoclaved aerated concrete prepared by utilizing waste FCC catalyst and preparation method thereof
CN112573863A (en) * 2019-09-29 2021-03-30 中国石油化工股份有限公司 Preparation method for improving intensity of geopolymer of catalytic cracking waste catalyst
CN114572994A (en) * 2022-02-28 2022-06-03 西藏大学 Zeolite-like material and preparation method and application thereof
CN114572994B (en) * 2022-02-28 2024-04-12 西藏大学 Zeolite-like material and its preparing process and application

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