CN111548044A - Activator for applying copper smelting waste residues in concrete and preparation method thereof - Google Patents
Activator for applying copper smelting waste residues in concrete and preparation method thereof Download PDFInfo
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- CN111548044A CN111548044A CN202010227734.9A CN202010227734A CN111548044A CN 111548044 A CN111548044 A CN 111548044A CN 202010227734 A CN202010227734 A CN 202010227734A CN 111548044 A CN111548044 A CN 111548044A
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- Prior art keywords
- concrete
- copper smelting
- activator
- smelting waste
- polyoxyethylene ether
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Classifications
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
-
- 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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/14—Waste materials; Refuse from metallurgical processes
- C04B18/141—Slags
- C04B18/144—Slags from the production of specific metals other than iron or of specific alloys, e.g. ferrochrome slags
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Civil Engineering (AREA)
- Health & Medical Sciences (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses an activator for applying copper smelting waste residue in concrete and a preparation method thereof. The preparation method of the activator has the advantages of mild process conditions, simple and easily-controlled equipment, high production efficiency, zero emission and no pollution; the produced novel active excited solid powder auxiliary agent has the advantages of convenient packaging and transportation, and easy mixing, grinding and adding with copper smelting waste residue. When the copper smelting waste residue with the activity excited by the activator is applied to concrete, the copper smelting waste residue can replace mineral powder and fly ash in the concrete and reduce the using amount of cement on the premise of ensuring the workability, strength and durability of the concrete, so that the waste is changed into valuable, and the problems of shortage of admixture supply and unstable quality required by green treatment of the copper smelting waste residue and concrete production are solved.
Description
Technical Field
The invention belongs to the field of green processing and resource utilization of industrial non-hazardous solid waste, and particularly relates to an activator for applying copper smelting waste residue in concrete and a preparation method thereof.
Background
With the improvement of environmental awareness and improvement of relevant regulations in China and the world, massive industrial solid wastes from mining, ore processing and mineral smelting face huge pressure and technical requirements for harmless treatment and resource utilization.
The huge demand of copper products in China promotes China to develop into a large copper smelting country, and the copper smelting yield value in 2018 is nearly 9000 million yuan and the copper smelting yield value in 2019 exceeds 9000 million yuan in China. Also associated with the enormous copper production is the production of millions of tons of copper smelting slags each year. The conventional method for disposing the copper smelting waste slag is landfill, but the method occupies a large amount of land and does not meet the environmental protection requirement of current social development due to secondary pollution; and a small amount of the slag is sold to nearby cement enterprises to be used as a cement production auxiliary material, or is used as a low-grade steelmaking raw material when the slag contains high iron content and nearby steel plants exist, but the consumption is very limited.
In recent years, the foundation construction of China is continuously promoted, the demand of concrete is steadily increased, natural sand is limited to mining and is forbidden to be mined, and machine-made sand gradually replaces natural sand, but the machine-made sand is generally thicker, and fine particles are urgently needed to supplement the shortage of fine aggregate gradation; on the other hand, with the gradual compression of thermal power plants and the replacement of the thermal power plants by new energy, steel plants are integrated, the fly ash and the mineral powder as the traditional admixture for the concrete cannot meet the requirements of the current concrete in terms of quantity and quality, the cost and the price of the fly ash respectively reach over 180 yuan/ton and 350 yuan/ton, the cost and the pressure of the concrete are continuously increased, and the seeking and the development of the novel admixture for the concrete for replacing the fly ash and the mineral powder and reducing the consumption of the cement are urgent.
Copper smelting waste slag is a solid mixture containing elements such as calcium, silicon, aluminum, iron, oxygen and the like, and the processing and modification of the copper smelting waste slag into a novel raw material for concrete production are not reported at present. According to the invention, the developed activator is used for processing the copper smelting waste residues into the composite admixture which can be directly applied to concrete, so that the problem of harmless treatment of a large amount of copper smelting solid wastes is solved, the dilemma that the existing concrete auxiliary cementing material is high in shortage price and insufficient in fine aggregate can be effectively relieved, the waste is really changed into valuable, and the key raw material with high cost performance is provided for important basic engineering such as national infrastructure and the like.
Disclosure of Invention
The invention provides an activator for applying copper smelting waste residues in concrete and a preparation method thereof, which solve the problem that solid waste generated by large amount of copper smelting is not friendly and effective to treat. The recycling problem of the copper smelting waste residue is solved, and the problem of mixing the waste residue and concrete is solved through a medicament.
In order to achieve the purpose, the invention provides the following technical scheme: an activator for copper smelting waste residue applied in concrete and a preparation method thereof, the active ingredient of the activator is triflate of which the total content is more than 90 percent and which is coordinated by sulfonic-group-rich polyoxyethylene ether and alcohol amine, and the preparation method comprises the following steps:
under normal pressure, heat-melting a polyoxyethylene ether monomer with the molecular weight of 1000-3000 in a stainless steel or enamel reaction kettle at the temperature of 50-70 ℃ for 30-90 minutes;
then, adding one or more of 5-10% by mass of double bond-containing sodium methallyl sulfonate, calcium methallyl sulfonate, 2-acrylamide-2-methylpropanesulfonic acid sodium salt and 2-acrylamide-2-methylpropanesulfonic acid calcium salt into the hot melt within 10-30 minutes under the stirring of 30-60 rpm;
then, weighing one or more of ammonium persulfate, sodium persulfate and potassium persulfate according to the mass fraction of 0.3-1.2% of the polyoxyethylene ether monomer, weighing one or more of polyethylene glycol 200, 400, 600, 800 and 1000 according to the mass fraction of 0.1-0.4% of the polyoxyethylene ether monomer, fully mixing the two into polyethylene glycol emulsion by using a premixing barrel with shearing and stirring, and adding the emulsion into the reaction kettle within 0.5-3.5 hours under the stirring of 30-60 rpm;
finally, weighing one or more of zinc trifluoromethanesulfonate, sodium trifluoromethanesulfonate and calcium trifluoromethanesulfonate according to the mass fraction of 2-5% of polyoxyethylene ether, weighing one or more of ethanolamine, diethanolamine and triethanolamine according to the mass fraction of 1-3% of polyoxyethylene ether, simultaneously adding the trifluoromethanesulfonate and the alkanolamine into the reaction system under the stirring of 30-60rpm, stirring for 30-120 minutes, pumping fluid into a storage tank with a screw shearing blade, and naturally cooling at normal pressure or negative pressure to obtain the novel auxiliary material which can excite the activity of the copper smelting waste residue and is applied to the concrete
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the activator for applying the copper smelting waste residue to the concrete has mild preparation process conditions, easy realization of equipment automation, high production efficiency, zero emission and no pollution; the synthesized activator has the advantages of convenient packaging and transportation, simple and convenient addition to copper smelting slag, and capability of effectively exciting copper smelting slag to become active admixture and active fine aggregate, and further being directly applied to concrete production to improve the workability, mechanical property and durability of concrete. The activator realizes the recycling of copper waste residue resources, saves energy, protects environment and simultaneously ensures the quality and the yield of concrete.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The embodiment provides an activator for applying copper smelting waste residue in concrete and a preparation method thereof. The activator comprises sulfonic group-rich polyoxyethylene ether with the total content of more than 90 percent and trifluoromethanesulfonate coordinated with alcohol amine.
The preparation method of the activator comprises the following steps:
a. according to the mass, 100 parts of polyoxyethylene ether monomer with the molecular weight of 1200 is hot-melted for 45 minutes in a stainless steel reaction kettle at the temperature of 58 ℃ under normal pressure;
b. stirring at the rotating speed of 42rpm, and adding 3 parts of calcium methallyl sulfonate and 2 parts of 2-acrylamide-2-methylpropanesulfonic acid sodium salt into the hot melt within 15 minutes;
c. fully mixing 0.8 part of sodium persulfate and 0.2 part of polyethylene glycol 600 into polyethylene glycol emulsion by shearing and stirring in a premixing barrel, and uniformly adding the emulsion into a reaction kettle within 2 hours under the stirring of 42 rpm;
d. weighing 3 parts of zinc trifluoromethanesulfonate and 1 part of ethanolamine, simultaneously adding the zinc trifluoromethanesulfonate and the ethanolamine into a reaction kettle while stirring at 42rpm, stirring for 90 minutes, pumping a product into a storage tank with screw shearing blades, and naturally cooling at normal pressure to obtain the activator which has 99.09% of effective solid content and is used for activating the copper smelting waste residues and applying the activator to concrete.
Adding the prepared activator into copper smelting waste residues according to 2 percent of the copper smelting waste residues, performing ball milling and screening by a 325-mesh sieve to obtain a composite admixture, wherein the composite admixture is applied to the production of concrete pumped by C30 per cubic meter, 210 kg of P.O.42.5 cement, 40 kg of secondary fly ash and 90 kg of the composite admixture derived from the copper smelting waste residues.
Example 2
The embodiment provides an activator for applying copper smelting waste residue in concrete and a preparation method thereof. The activator comprises sulfonic group-rich polyoxyethylene ether with the total content of more than 90 percent and trifluoromethanesulfonate coordinated with alcohol amine.
The preparation method of the activator comprises the following steps:
a. according to the mass, 100 parts of polyoxyethylene ether monomer with the molecular weight of 2400 is hot-melted in a ceramic reaction kettle at the temperature of 65 ℃ for 60 minutes under normal pressure;
b. stirring at the rotating speed of 51rpm, and adding 3 parts of calcium methallyl sulfonate and 3 parts of 2-acrylamide-2-methylpropanesulfonic acid sodium into the hot melt within 30 minutes;
c. 1.2 parts of sodium persulfate and 0.3 part of polyethylene glycol 200 are fully mixed into polyethylene glycol emulsion by shearing and stirring in a premixing barrel, and the emulsion is uniformly added into a reaction kettle within 3 hours under the stirring of 51 rpm;
d. weighing 5 parts of zinc trifluoromethanesulfonate and 2 parts of diethanolamine, simultaneously adding the zinc trifluoromethanesulfonate and the diethanolamine into a reaction kettle while stirring at 51rpm, stirring for 120 minutes, pumping a product into a storage tank with a screw shear blade, and naturally cooling at normal pressure to obtain the activator which has 99.73% of effective solid content and is used for activating the copper smelting waste residue and applying the activator to concrete.
Adding the prepared activator into copper smelting waste residues according to 5 percent of the copper smelting waste residues, performing ball milling and screening by a 325-mesh sieve to obtain a composite admixture, wherein 200 kg of the activator is used for producing P.O.42.5 cement per cubic C30 pump concrete, 50 kg of secondary fly ash is used, and 100 kg of the composite admixture derived from the copper smelting waste residues is used.
Example 3
The embodiment provides an activator for applying copper smelting waste residue in concrete and a preparation method thereof. The activator comprises sulfonic group-rich polyoxyethylene ether with the total content of more than 90 percent and trifluoromethanesulfonate coordinated with alcohol amine.
The preparation method of the activator comprises the following steps:
a. according to mass, 100 parts of polyoxyethylene ether monomer with the molecular weight of 2200 is hot-melted for 90 minutes in a ceramic reaction kettle at 70 ℃ under normal pressure;
b. stirring at the rotating speed of 60rpm, and adding 5 parts of calcium methallyl sulfonate and 5 parts of 2-acrylamide-2-methylpropanesulfonic acid sodium into the hot melt within 20 minutes;
c. 1.0 part of sodium persulfate and 0.2 part of polyethylene glycol 800 are fully mixed into polyethylene glycol emulsion by shearing and stirring in a premixing barrel, and the emulsion is uniformly added into a reaction kettle within 3.5 hours under the stirring of 60 rpm;
d. weighing 3 parts of zinc trifluoromethanesulfonate and 3 parts of triethanolamine, adding the zinc trifluoromethanesulfonate and the triethanolamine into a reaction kettle while stirring at 60rpm, stirring for 90 minutes, pumping the product into a storage tank with a screw shearing blade, and naturally cooling at normal pressure to obtain the activator which has 99.83% of effective solid content and is used for exciting the activity of the copper smelting waste residue and is applied to concrete.
Adding the prepared activator into copper smelting waste residue according to 10 percent of the copper smelting waste residue, performing ball milling and screening by a 325-mesh sieve to obtain a composite admixture, and applying the composite admixture to the production of concrete pumped by C30 per cubic meter, wherein 180 kilograms of P, II, 52.5 cement is used, 50 kilograms of secondary fly ash is used, and 120 kilograms of the composite admixture derived from the copper smelting waste residue is used.
Example 4
To verify the effects of the activators obtained in examples 1, 2 and 3, concrete experiments were carried out, the contents of which are described in examples 1, 2 and 3, and the results of which are shown in the following table.
| Species of | Initial slump/spread | Slump/spread after 1h | Compressive strength of 7 days | 28 day compressive strength |
| Example 1 | 220/580mm | 205/560mm | 26.2MPa | 37.5MPa |
| Example 2 | 205/562mm | 200/545mm | 28.1MPa | 39.7MPa |
| Example 3 | 215/570mm | 210/555mm | 29.5MPa | 41.6MPa |
| Standard value | Not less than 160/450mm | Not less than 160/450mm | Not less than 22.5MPa | Not less than 34.5MPa |
The data values of the examples in the table are compared with the standard values, and the results obtained by concrete experiments of the examples 1, 2 and 3 all meet the design requirements of concrete.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. An activator for applying copper smelting waste residue in concrete is characterized in that the activator comprises sulfonic acid-rich polyoxyethylene ether with the total content of more than 90% and triflate coordinated by alcohol amine.
2. A method for preparing the activator for the application of the copper smelting waste slag in concrete according to claim 1, which is characterized by comprising the following steps:
(1) at normal pressure and 50-70 ℃, the polyoxyethylene ether monomer is hot melted;
(2) adding double bond-containing sulfonate into the hot melt, and continuously stirring to uniformly disperse the sulfonate;
(3) adding the persulfate polyethylene glycol emulsion which is quickly sheared and uniformly stirred into a reaction kettle while stirring within 0.5-3.5 hours;
(4) adding the triflate and the alcohol amine into the system in the last step at the same time, stirring for 30-120 minutes, pumping the fluid into a storage tank with a screw shearing blade, and naturally cooling at normal pressure or negative pressure.
3. The method of claim 2, wherein: the double-bond sulfonate is one or more of sodium methallylsulfonate, calcium methallylsulfonate, 2-acrylamide-2-methylpropanesulfonic acid sodium and 2-acrylamide-2-methylpropanesulfonic acid calcium; the using amount of the sulfonate containing double bonds is 5-10% of the mass fraction of the polyoxyethylene ether monomer.
4. The method of claim 2, wherein: the polyethylene glycol refers to one or more of polyethylene glycol 200, 400, 600, 800 and 1000; the dosage of the polyethylene glycol is 0.1-0.4% of the mass fraction of the polyoxyethylene ether monomer.
5. The method of claim 2, wherein: the persulfate is one or more of ammonium persulfate, sodium persulfate and potassium persulfate; the consumption of the persulfate is 0.3-1.2% of the mass fraction of the polyoxyethylene ether monomer.
6. The method of claim 2, wherein: the trifluoromethanesulfonate is one or more of zinc trifluoromethanesulfonate, sodium trifluoromethanesulfonate and calcium trifluoromethanesulfonate; the amount of the triflate is 2-5% of the mass fraction of the polyoxyethylene ether monomer.
7. The method of claim 2, wherein: the alcohol amine refers to one or more of ethanolamine, diethanolamine and triethanolamine; the using amount of the alcohol amine is 1-3% of the mass fraction of the polyoxyethylene ether monomer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010227734.9A CN111548044B (en) | 2020-03-27 | 2020-03-27 | Activator for applying copper smelting waste residues in concrete and preparation method thereof |
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| CN202010227734.9A CN111548044B (en) | 2020-03-27 | 2020-03-27 | Activator for applying copper smelting waste residues in concrete and preparation method thereof |
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| CN111548044A true CN111548044A (en) | 2020-08-18 |
| CN111548044B CN111548044B (en) | 2021-04-02 |
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Citations (6)
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|---|---|---|---|---|
| GB2382303B (en) * | 2000-07-31 | 2004-12-01 | Johnson & Son Inc S C | Low residue surface treatment |
| CN101717837A (en) * | 2009-12-19 | 2010-06-02 | 中北大学 | Chemical activation liquid of converter slag and application method thereof |
| CN103316566A (en) * | 2013-06-21 | 2013-09-25 | 绍兴文理学院 | Hydramine and trifluoromethanesulfonic acid alkali metal salt combination solution as well as preparation method and application thereof |
| CN103693886A (en) * | 2013-12-19 | 2014-04-02 | 聊城大学 | Slag compound activating grinding aid and preparation method thereof |
| CN104028385A (en) * | 2014-06-16 | 2014-09-10 | 山东科技大学 | Preparation method of coal slime flotation accelerant and coal slime flotation method |
| CN106915910A (en) * | 2017-03-31 | 2017-07-04 | 王秀贵 | A kind of activity excitant of nonactive volcanic ash and preparation method thereof |
-
2020
- 2020-03-27 CN CN202010227734.9A patent/CN111548044B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2382303B (en) * | 2000-07-31 | 2004-12-01 | Johnson & Son Inc S C | Low residue surface treatment |
| CN101717837A (en) * | 2009-12-19 | 2010-06-02 | 中北大学 | Chemical activation liquid of converter slag and application method thereof |
| CN103316566A (en) * | 2013-06-21 | 2013-09-25 | 绍兴文理学院 | Hydramine and trifluoromethanesulfonic acid alkali metal salt combination solution as well as preparation method and application thereof |
| CN103693886A (en) * | 2013-12-19 | 2014-04-02 | 聊城大学 | Slag compound activating grinding aid and preparation method thereof |
| CN104028385A (en) * | 2014-06-16 | 2014-09-10 | 山东科技大学 | Preparation method of coal slime flotation accelerant and coal slime flotation method |
| CN106915910A (en) * | 2017-03-31 | 2017-07-04 | 王秀贵 | A kind of activity excitant of nonactive volcanic ash and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张巨松等: "《混凝土原材料》", 31 January 2019 * |
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