CN103880310A - Portland blast furnace slag cement and preparation method thereof - Google Patents

Portland blast furnace slag cement and preparation method thereof Download PDF

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Publication number
CN103880310A
CN103880310A CN201410057747.0A CN201410057747A CN103880310A CN 103880310 A CN103880310 A CN 103880310A CN 201410057747 A CN201410057747 A CN 201410057747A CN 103880310 A CN103880310 A CN 103880310A
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slag
cement
portland
furnace slag
blast furnace
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CN103880310B (en
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周宇飞
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Liaoning Petrochemical Vocational and Technical College
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    • 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
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/10Production of cement, e.g. improving or optimising the production methods; Cement grinding

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Abstract

The invention relates to a portland blast furnace slag cement and a preparation method thereof. The portland blast furnace slag cement is prepared from the following raw materials by weight percent: 12%-30% of at least one of slag, coal gangue, boiling slag, liquid slag, cinerite, kiln dust and crushed tile, 10%-42% of mineral waste residue, steel slag or silicomanganese slag, 0-12% of limestone, 2%-8% of gypsum, 0-10% of zeolite, 0-17% of boiling slag, 0-10% of coal ash, and 10%-50% of silicate series cement. The preparation method comprises steps of putting the slag, mineral waste residue, gypsum, zeolite, boiling slag, and coal ash into a pulverizer to be smashed, grinding by a ball mill to achieve the fineness of 0.08mm, sieving by a square hole sieve with 2% left, and then mixing with the silicate series cement. The portland blast furnace slag cement has the advantages of having a simple preparation method, needing no cement clinker, guaranteeing the strength and stability of the cement, fully using industrial residue resources like slag and mineral waste residue, lowering production cost, and reducing the pollution of industrial residue to the environment.

Description

A kind of Portland blast furnace slag cement and production method thereof
Technical field
The present invention relates to a kind of Portland blast furnace slag cement and production method thereof.
Background technology
The production technique of existing cement is all first to produce cement clinker, by crude fuel: Wingdale, iron powder, clay, coal gangue, shale, gypsum, fluorite and coal etc. on request proportioning carry out grinding, reach after certain fineness, produce work in-process---cement clinker through calcining, then admixture different sorts blended material and gypsum, carry out grinding for the second time, make it reach certain fineness, just become finished product---cement.The disadvantage that this method is produced cement is to have grog to produce this link, and in clinker burning process, consumes mass energy, environment is caused to serious pollution simultaneously, and production process complexity, and quality product fluctuation is larger.In addition, there are many areas not exist and produce grog condition, if any fuel but without Wingdale, but have Wingdale without fuel.There are a large amount of blended materials in some areas, and as the waste residue of ironworks, ferroalloy works, Steel Plant's discharge, pile up like a mountain, can not utilize.The mountain area having again stores a large amount of Zeolite Rock classes, ash rock class, but lacks grog working condition and can not produce cement.Northern area winter, heating was used a large amount of fire coals, produced a large amount of slag ash, except small part is done some insulation and baked bricks, be emitted in a large number in the Nature, and not only contaminate environment, also land occupation resource, is a very large waste.And the cement that these areas need ships from far place again, price is very high, has both increased building cost, causes again the waste of the energy and resource.
Summary of the invention
It is simple that the technical problem to be solved in the present invention is to provide a kind of technique, do not need cement clinker, ensureing under the prerequisite of strength of cement and stability, make full use of the industrial residue such as slag, slag resource, reduce production costs, reduce Portland blast furnace slag cement and the production method thereof of industrial residue environmental pollution.
Technical solution of the present invention is:
A kind of Portland blast furnace slag cement, is made up of following raw material by weight percentage:
In slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one 12%~30%;
Slag, slag or silicon manganese slag 10%~42%;
Wingdale 0~12%;
Gypsum 2%~8%;
Zeolite 0~10%;
Boiling furnace slag 0~17%;
Flyash 0~10%;
Silicate series cement 10%~50%.
Described Portland blast furnace slag cement, is made up of following raw material by weight percentage:
In slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one 15%~30%;
Slag, slag or silicon manganese slag 30%~42%;
Wingdale 7%~12%;
Gypsum 2%~8%;
Zeolite 5%~10%;
Boiling furnace slag 0~17%;
Flyash 7%~10%;
Silicate series cement 10%~30%.
Described silicate series cement is at least one in silicate cement, ordinary Portland cement, Portland blast furnace slag cement, portland-pozzolan cement, Portland fly ash cement, composite Portland cement, quick hardening Portland cement.
Described slag is granulated blast-furnace slag; Described flyash is III level flyash.
Described gypsum is at least one in dihydrate gypsum, saline gypsum, phosphogypsum, dehydrated gyp-, bassanite.
A production method for Portland blast furnace slag cement, its concrete steps are as follows:
By be respectively by weight percent in 12%~30% slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one, after 10%~42% slag, slag or silicon manganese slag, 0~12% Wingdale, 2%~8% gypsum, 0~10% zeolite, 0~17% boiling furnace slag, 0~10% flyash sends into pulverizer and pulverizes, be that 0.08mm square hole sieve tails over below 2% through ball mill grinding to fineness, mix with 10%~50% silicate series cement again, obtain Portland blast furnace slag cement.
Described Portland blast furnace slag cement is by weight percentage: in slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one 15%~30%; Slag, slag or silicon manganese slag 30%~42%; Wingdale 7%~12%; Gypsum 2%~8%; Zeolite 5%~10%; Boiling furnace slag 0~17%; Flyash 7%~10%; Silicate series cement 10%~30%.
Described silicate series cement is at least one in silicate cement, ordinary Portland cement, Portland blast furnace slag cement, portland-pozzolan cement, Portland fly ash cement, composite Portland cement, quick hardening Portland cement.
Described slag is granulated blast-furnace slag; Described flyash is III level flyash.
Described gypsum is at least one in dihydrate gypsum, saline gypsum, phosphogypsum, dehydrated gyp-, bassanite.
Beneficial effect of the present invention:
1, taking silicate cement 32.5,42.5,52.5 as feed composition, then mix the slag and the slag etc. that meet manufacture of cement condition, reduced production cost, reduced environmental pollution.Adopt gypsum, unslaked lime to excite, with the active SiO in raw material 2and Al 2o 3effect, plays the effect of stimulating activity; Owing to mixing zeolite, the fCaO that easily causes the cracking of cement in flyash is changed into the exciting agent that improves strength of cement, make soundness fabulous.
2, do not need cement clinker, can reach significant save energy, reduce the effect of environmental pollution, the add-on of the industrial residue such as slag and slag can be used at most 50% left and right, solve industrial residue in conventional art and can add-on only have 20% left and right, the problem that industrial residue utilization rate is low, has greatly saved Nonrenewable resources, reduces the pollution of industrial residue to environment; The strength of cement of producing is identical with raw materials used cement or exceed former label, belongs to low alkalinity cement, and sulfate resistance erosion and leakage resistance are strong, and its over-all properties exceedes the impervious, cement of existing kind.
3, technique is simple, forms through pulverizing ground and mixed taking the industrial residue such as slag, slag and cement as raw material, and raw material is easy to get, with low cost, has reduced grog production unit and has dropped into, and is applicable to large-scale cement grinding station suitability for industrialized production.
4, reduce production costs, compared with prior art, 15% left and right can reduce production costs.
Embodiment
Embodiment 1
Take 12kg slag, 35kg granulated blast-furnace slag, 12kg Wingdale, 6kg dihydrate gypsum, 5kg zeolite, 13kg boiling furnace slag, 7kg III level flyash; send into after pulverizer pulverizing; be that 0.08mm square hole sieve tails over below 2% through ball mill grinding to fineness; mix with the Portland blast furnace slag cement (32.5 Portland blast furnace slag cement) of 10kg again, obtain 32.5 Portland blast furnace slag cements.
Embodiment 2
Take 20kg slag, 42kg granulated blast-furnace slag, 2kg dehydrated gyp-, 9kg zeolite, 17kg boiling furnace slag; send into after pulverizer pulverizing; be that 0.08mm square hole sieve tails over below 2% through ball mill grinding to fineness; mix with the Portland blast furnace slag cement (32.5 Portland blast furnace slag cement) of 10kg again, obtain 32.5 Portland blast furnace slag cements.
Embodiment 3
Take 30kg slag, 10kg granulated blast-furnace slag, 7kg Wingdale, 3kg phosphogypsum, 10kg zeolite, 10kg III level flyash; send into after pulverizer pulverizing; be that 0.08mm square hole sieve tails over below 2% through ball mill grinding to fineness; mix with the Portland blast furnace slag cement (42.5 Portland blast furnace slag cement) of 30kg again, obtain 42.5 Portland blast furnace slag cements.
Embodiment 4
Taking 15kg coal gangue, 30kg silicon manganese slag, 7kg Wingdale, 8kg saline gypsum, 5kg boiling furnace slag, 5kg III level flyash, send into after pulverizer pulverizing, is that 0.08mm square hole sieve tails over below 2% through ball mill grinding to fineness; Mix with the Portland blast furnace slag cement (42.5 Portland blast furnace slag cement) of 30kg again, obtain 42.5 Portland blast furnace slag cements.
Silicate cement in embodiment 1~embodiment 4 can use ordinary Portland cement, Portland blast furnace slag cement, portland-pozzolan cement, Portland fly ash cement, composite Portland cement or quick hardening Portland cement to substitute; Slag in embodiment 1~embodiment 4 can use coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash or broken brick and tile to substitute; Granulated blast-furnace slag in embodiment 1~embodiment 4 can substitute with slag or silicon manganese slag; Dihydrate gypsum, saline gypsum, phosphogypsum, dehydrated gyp-and bassanite in embodiment 1~embodiment 4 can phase trans-substitution.
The detection results of property of the Portland fly ash cement of the embodiment of the present invention 1~embodiment 4 is as shown in table 1.
Table 1
Figure 868359DEST_PATH_IMAGE001

Claims (10)

1. a Portland blast furnace slag cement, is characterized in that: be made up of following raw material by weight percentage:
In slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one 12%~30%;
Slag, slag or silicon manganese slag 10%~42%;
Wingdale 0~12%;
Gypsum 2%~8%;
Zeolite 0~10%;
Boiling furnace slag 0~17%;
Flyash 0~10%;
Silicate series cement 10%~50%.
2. require the Portland blast furnace slag cement described in 1 according to power, it is characterized in that: formed by following raw material by weight percentage:
In slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one 15%~30%;
Slag, slag or silicon manganese slag 30%~42%;
Wingdale 7%~12%;
Gypsum 2%~8%;
Zeolite 5%~10%;
Boiling furnace slag 0~17%;
Flyash 7%~10%;
Silicate series cement 10%~30%.
3. require the Portland blast furnace slag cement described in 1 or 2 according to power, it is characterized in that: described silicate series cement is at least one in silicate cement, ordinary Portland cement, Portland blast furnace slag cement, portland-pozzolan cement, Portland fly ash cement, composite Portland cement, quick hardening Portland cement.
4. require the Portland blast furnace slag cement described in 1 or 2 according to power, it is characterized in that: described slag is granulated blast-furnace slag; Described flyash is III level flyash.
5. require the Portland blast furnace slag cement described in 1 or 2 according to power, it is characterized in that: described gypsum is at least one in dihydrate gypsum, saline gypsum, phosphogypsum, dehydrated gyp-, bassanite.
6. a production method for Portland blast furnace slag cement, is characterized in that: concrete steps are as follows:
By be respectively by weight percent in 12%~30% slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one, after 10%~42% slag, slag or silicon manganese slag, 0~12% Wingdale, 2%~8% gypsum, 0~10% zeolite, 0~17% boiling furnace slag, 0~10% flyash sends into pulverizer and pulverizes, be that 0.08mm square hole sieve tails over below 2% through ball mill grinding to fineness, mix with 10%~50% silicate series cement again, obtain Portland blast furnace slag cement.
7. the production method of Portland blast furnace slag cement according to claim 6, is characterized in that: by weight percentage: in slag, coal gangue, boiling furnace slag, liquid slag, volcanic ash, kiln ash, broken brick and tile at least one 15%~30%; Slag, slag or silicon manganese slag 30%~42%; Wingdale 7%~12%; Gypsum 2%~8%; Zeolite 5%~10%; Boiling furnace slag 0~17%; Flyash 7%~10%; Silicate series cement 10%~30%.
8. according to the production method of the Portland blast furnace slag cement described in claim 6 or 7, it is characterized in that: described silicate series cement is at least one in silicate cement, ordinary Portland cement, Portland blast furnace slag cement, portland-pozzolan cement, Portland fly ash cement, composite Portland cement, quick hardening Portland cement.
9. according to the production method of the Portland blast furnace slag cement described in claim 6 or 7, it is characterized in that: described slag is granulated blast-furnace slag; Described flyash is III level flyash.
10. according to the production method of the Portland blast furnace slag cement described in claim 6 or 7, it is characterized in that: described gypsum is at least one in dihydrate gypsum, saline gypsum, phosphogypsum, dehydrated gyp-, bassanite.
CN201410057747.0A 2014-02-20 2014-02-20 A kind of portland slag cement and production method thereof Expired - Fee Related CN103880310B (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104788029A (en) * 2015-03-23 2015-07-22 苏州市德莱尔建材科技有限公司 Rapid hardening Portland cement and preparation method thereof
CN105481335A (en) * 2015-12-22 2016-04-13 乐陵市恒鑫新型建材有限公司 Baking-free brick taking silicon-manganese slag and pulverized fuel ash as main materials
CN105776907A (en) * 2014-12-24 2016-07-20 嘉华特种水泥股份有限公司 Special air-setting hydraulic Portland cement for wet-mixed mortar
CN105837148A (en) * 2016-03-26 2016-08-10 南京兰叶建设集团有限公司 Waste residue cement
CN106242329A (en) * 2016-07-20 2016-12-21 山东东华水泥有限公司 A kind of cement grinding process
CN107867805A (en) * 2017-11-30 2018-04-03 柳州市郊区和平第五砖厂 A kind of high strength cement and preparation method thereof
CN107922265A (en) * 2015-06-29 2018-04-17 罗马水泥有限责任公司 Pozzolanic material performance it is mixed and modified
CN107986648A (en) * 2017-12-26 2018-05-04 天津山水水泥有限公司 Portland slag cement and preparation method thereof
CN108609875A (en) * 2018-05-15 2018-10-02 鞍钢股份有限公司 A method of preparing cement admixture using vessel slag
CN109626900A (en) * 2018-12-26 2019-04-16 福建源鑫建材有限公司 A kind of portland slag cement and its production method
CN111268928A (en) * 2020-02-28 2020-06-12 桂林理工大学 Composite micro powder partially replacing cement and cement-based material
CN111302676A (en) * 2018-12-11 2020-06-19 福州金牛水泥有限公司 Method for adding slag micro powder in cement and concrete
CN111348847A (en) * 2020-04-08 2020-06-30 常朋朋 Cement and preparation method thereof
CN111499236A (en) * 2020-05-08 2020-08-07 张延年 Production method for preparing portland cement by using large-amount fly ash and chemical gypsum
CN114292045A (en) * 2021-10-11 2022-04-08 湖南绿生永固新材料有限公司 Green concrete admixture of silicomanganese smelting slag and preparation method thereof
CN115321849A (en) * 2022-08-04 2022-11-11 四川利森建材集团有限公司 Silicomanganese slag limestone composite low-carbon cementing material and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101182139A (en) * 2007-11-12 2008-05-21 华南理工大学 Masonry cement having higher strength and water retention

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101182139A (en) * 2007-11-12 2008-05-21 华南理工大学 Masonry cement having higher strength and water retention

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105776907A (en) * 2014-12-24 2016-07-20 嘉华特种水泥股份有限公司 Special air-setting hydraulic Portland cement for wet-mixed mortar
CN105776907B (en) * 2014-12-24 2018-09-07 嘉华特种水泥股份有限公司 A kind of solidifying property portland cement of the special air condensate of wet mixing mortar
CN104788029A (en) * 2015-03-23 2015-07-22 苏州市德莱尔建材科技有限公司 Rapid hardening Portland cement and preparation method thereof
CN107922265A (en) * 2015-06-29 2018-04-17 罗马水泥有限责任公司 Pozzolanic material performance it is mixed and modified
CN105481335A (en) * 2015-12-22 2016-04-13 乐陵市恒鑫新型建材有限公司 Baking-free brick taking silicon-manganese slag and pulverized fuel ash as main materials
CN105837148A (en) * 2016-03-26 2016-08-10 南京兰叶建设集团有限公司 Waste residue cement
CN106242329A (en) * 2016-07-20 2016-12-21 山东东华水泥有限公司 A kind of cement grinding process
CN107867805A (en) * 2017-11-30 2018-04-03 柳州市郊区和平第五砖厂 A kind of high strength cement and preparation method thereof
CN107986648A (en) * 2017-12-26 2018-05-04 天津山水水泥有限公司 Portland slag cement and preparation method thereof
CN108609875A (en) * 2018-05-15 2018-10-02 鞍钢股份有限公司 A method of preparing cement admixture using vessel slag
CN111302676A (en) * 2018-12-11 2020-06-19 福州金牛水泥有限公司 Method for adding slag micro powder in cement and concrete
CN109626900A (en) * 2018-12-26 2019-04-16 福建源鑫建材有限公司 A kind of portland slag cement and its production method
CN111268928A (en) * 2020-02-28 2020-06-12 桂林理工大学 Composite micro powder partially replacing cement and cement-based material
CN111348847A (en) * 2020-04-08 2020-06-30 常朋朋 Cement and preparation method thereof
CN111499236A (en) * 2020-05-08 2020-08-07 张延年 Production method for preparing portland cement by using large-amount fly ash and chemical gypsum
CN114292045A (en) * 2021-10-11 2022-04-08 湖南绿生永固新材料有限公司 Green concrete admixture of silicomanganese smelting slag and preparation method thereof
CN115321849A (en) * 2022-08-04 2022-11-11 四川利森建材集团有限公司 Silicomanganese slag limestone composite low-carbon cementing material and application thereof
CN115321849B (en) * 2022-08-04 2023-09-22 四川利森建材集团有限公司 Silicon-manganese slag-limestone composite low-carbon gelling material and application thereof

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