CN114685070A - Preparation method of novel boron-containing sulphoaluminate cementing material and radiation-proof cementing material obtained by preparation method - Google Patents
Preparation method of novel boron-containing sulphoaluminate cementing material and radiation-proof cementing material obtained by preparation method Download PDFInfo
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- CN114685070A CN114685070A CN202011645637.8A CN202011645637A CN114685070A CN 114685070 A CN114685070 A CN 114685070A CN 202011645637 A CN202011645637 A CN 202011645637A CN 114685070 A CN114685070 A CN 114685070A
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- boron
- cementing material
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- sulphoaluminate
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000004568 cement Substances 0.000 claims abstract description 51
- 239000010440 gypsum Substances 0.000 claims abstract description 20
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 5
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 235000019738 Limestone Nutrition 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000006028 limestone Substances 0.000 claims abstract description 3
- 238000005245 sintering Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007790 solid phase Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 claims description 4
- 229910021538 borax Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 230000005855 radiation Effects 0.000 claims description 4
- 239000004328 sodium tetraborate Substances 0.000 claims description 4
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 239000002989 correction material Substances 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims 1
- 235000012211 aluminium silicate Nutrition 0.000 claims 1
- QYHKLBKLFBZGAI-UHFFFAOYSA-N boron magnesium Chemical compound [B].[Mg] QYHKLBKLFBZGAI-UHFFFAOYSA-N 0.000 claims 1
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims 1
- 239000010881 fly ash Substances 0.000 claims 1
- 239000004615 ingredient Substances 0.000 claims 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 7
- 239000004566 building material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 11
- 238000012360 testing method Methods 0.000 description 6
- 229910052788 barium Inorganic materials 0.000 description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 5
- 229910052712 strontium Inorganic materials 0.000 description 5
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 5
- 150000004683 dihydrates Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000006703 hydration reaction Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 239000011398 Portland cement Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C04B7/32—Aluminous cements
- C04B7/323—Calcium aluminosulfate cements, e.g. cements hydrating into ettringite
-
- 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
- C04B7/36—Manufacture of hydraulic cements in general
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to the field of special building material preparation, and particularly relates to a preparation method of a novel boron-containing sulphoaluminate cementing material and an obtained radiation-proof cementing material. The method comprises the following steps: grinding limestone and bauxite to below 180 meshes, drying, calculating the proportion of raw materials, introducing a boron-containing chemical, fully reacting at high temperature, rapidly cooling to normal temperature, and grinding the clinker and gypsum together to obtain the novel boron-containing sulphoaluminate cementing material with the sieved residue of 45 mu m below 25%. According to the method, in the solid phase reaction of the sulphoaluminate cement, a boron-containing compound is added, the content of the B element is controlled within a proper range of the components of the cement clinker, and the content of the B element is improved on the premise of not influencing the service performance of the sulphoaluminate cement, so that the novel boron-containing sulphoaluminate cement with the ray shielding capability is obtained.
Description
Technical Field
The invention belongs to the technical field of special building material preparation, and particularly relates to a preparation method of a novel boron-containing sulphoaluminate cementing material and an obtained radiation-proof cementing material.
Background
Nuclear power utilization is an important mark for national comprehensive national force and national defense strength, and is an important channel or means for relieving the energy crisis in China. When using nuclear energy, various safeguards are required to avoid serious consequences of nuclear radiation or nuclear leakage. Therefore, when building nuclear islands, nuclear protection projects and other buildings containing radioactive sources are built, various radiation-proof materials are required to be used for making full protection measures. The radiation-proof cement can ensure the safe operation of the nuclear reactor, weaken or absorb the energy of radiation, reduce the potential safety hazard existing in the nuclear utilization process and effectively protect the safety of human health and ecological environment.
The radiation-proof cement is not only an important cementing material, but also a functional protective material, and can be used in the projects of industrial flaw detection, agricultural breeding, scientific experiments, medical facilities, geological detection, nuclear waste solidification and the like. The radiation-proof cement commonly used at present comprises ordinary portland cement, barium cement, strontium cement, boron cement, high-alumina cement and the like.
But the existing radiation-proof cement still exists: (1) the absorption effect is not high: the existing various radiation-proof cements have poor radiation-absorbing effect, barium cement and strontium cement only have good X and gamma ray shielding effect, boron cement only has good neutron absorbing effect, and extra shielding additives are required to be added in the actual use process; (2) the preparation process and method have problems: the calcination temperature of the traditional barium cement and strontium cement is above 1550 ℃, and the energy consumption is huge. The boron cement is prepared by adding a boron-containing additive, borax has strong retarding effect, 4.5% of boric acid and 2% of borax are used as additives, and the setting time of the boron cement reaches 47 hours; (3) the shielding performance is difficult to be compatible with other performances: barium cement and strontium cement have poor thermal stability, and the hydration structure is seriously damaged at 100 ℃, so that the barium cement and the strontium cement can only be used in low-temperature environment. Under the irradiation condition of boron element in the traditional boron cement, boron cement products are easy to expand and crack. The high-alumina cement has high hydration rate and high hydration heat.
Disclosure of Invention
Aiming at the defects of the existing radiation-proof cement, the invention aims to provide a preparation method of a novel boron-containing sulphoaluminate cementing material and a radiation-proof cementing material obtained by the preparation method. According to the method, a boron-containing compound is added into a sulphoaluminate cement raw material system, the B element is solidified into cement clinker by utilizing the principle that the B element reacts with elements such as Mg, Ca and the like to generate a mineral phase, the content of the B element is controlled within a proper range of the components of the cement clinker, the B element is fully reacted by a high-temperature solid-phase sintering method, then air-cooled and rapidly cooled to normal temperature, and a proper amount of gypsum is added and ground to the corresponding fineness to obtain the novel boron-containing sulphoaluminate cementing material.
The technical scheme provided by the invention is as follows:
a preparation method of a novel boron-containing sulphoaluminate cementing material comprises the following steps:
preparing materials: the content range of the mineral phases of the clinker is designed by calculation as follows: c4 A3S%: 45-65%, C2S%: 30-50%, C4 AF%: 5%, M3B%: 0 to 10 percent. The raw materials are mixed, evenly mixed and tabletted, and then the mixture is dried with external water at 105 ℃.
And (3) calcining: calcining the raw material cake prepared in the step 1 under a calcination system corresponding to different components, wherein the calcination temperature ranges are as follows: 1300 ℃ and 1350 ℃, and the heat preservation time is 20-50 min. Primarily crushing the calcined raw material in one step, controlling the particle size to be 2-10mm, and then crushing in two steps, controlling the particle size to be below 1 mm.
Preparing cement: and (3) adding a proper amount of gypsum into the cement clinker crushed in the second step in the step (2), and placing the cement clinker into a horizontal ball mill for final grinding until the grain size is controlled to be 45 mu m, the screen residue is less than 25%, and the specific surface area is 400 +/-20 m2/kg, so as to obtain a final cement finished product, namely the novel boron-containing sulphoaluminate cementing material.
The raw materials used in the step 1 mainly comprise limestone and bauxite, the aluminum correction material is chemically pure alumina, the sulfur material is gypsum, and the boron-containing compound is selected from boric anhydride, borax and ascharite. The tabletting size is controlled to be phi 30x10 +/-3 mm, and the content range of clinker of each component is as follows: CaO%: 40-50%, Al2O 3%: 23-33%, SiO 2%: 9-17%, SO 3%: 5-9%, MgO%: 1-7%, B2O 3%: 0.9 to 4 percent.
The calcination system selected in the step 2 is the optimal calcination system designed according to each group of formulation ratio, and the calcined clinker is taken out, immediately cooled by air, quenched to normal temperature and crushed.
The gypsum in the step 3 is dihydrate gypsum, and after the dihydrate gypsum is added, the setting time of the sulphoaluminate cement can be prolonged properly, and the dihydrate gypsum also participates in the hydration reaction process, and the content of the dihydrate gypsum is controlled within a proper range.
Compared with the traditional boron cement, the boron-containing sulphoaluminate cement prepared by the boron-containing compound internal doping method has the advantages of lower calcination temperature, more energy conservation and environmental protection, and the high early strength of sulphoaluminate cement enables the boron-containing sulphoaluminate cement to have higher early strength, shorter setting time and more convenient engineering application compared with the common boron cement.
The invention also provides the low-cost cementing material produced by the production method.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1
Design C4A 3S% -45%, C2S% -50%, C4 AF% -5%, and M3B%: 0-10 percent, calculating the content of each required raw material, then weighing and proportioning, uniformly mixing and tabletting, wherein the size is phi 30x10 +/-3 mm, and drying in a drying box at 105 ℃.
Placing the prepared raw materials into a crucible, placing the crucible into a high-temperature furnace, calcining the raw materials to perform high-temperature solid-phase reaction, wherein the optimal reaction temperature is as follows: the optimal heat preservation time is as follows: and (5) 50 min.
After the high-temperature solid-phase sintering process is finished, taking out the clinker, air-cooling and quenching to normal temperature, carrying out one-step and two-step crushing, then weighing a proper amount of gypsum according to the mass percentage of clinker to gypsum of 90: 10, and placing the weighed gypsum in a horizontal ball mill for preparing cement.
And testing the mechanical properties of the prepared cement according to the standard.
The determination result shows that the novel boron-containing sulphoaluminate cementing material provided by the embodiment meets the requirement of strength grade 42.5.
Example 2
Design C4A 3S% -55%, C2S% -40%, C4 AF% -5%, and M3B%: 0-10 percent, calculating the content of each required raw material, then weighing and proportioning, uniformly mixing and tabletting, wherein the size is phi 30x10 +/-3 mm, and drying in a drying box at 105 ℃.
Placing the prepared raw materials into a crucible, placing the crucible into a high-temperature furnace, calcining the raw materials to perform high-temperature solid-phase reaction, wherein the optimal reaction temperature is as follows: the optimal heat preservation time is as follows at 1300 ℃: and (5) 50 min.
After the high-temperature solid-phase sintering process is finished, the clinker is taken out, air-cooled and quenched to normal temperature, one-step and two-step crushing is carried out, then a proper amount of gypsum is weighed according to the mass percentage of clinker to gypsum of 90: 10, and the mixture is placed in a horizontal ball mill for cement preparation.
And testing the mechanical properties of the prepared cement according to the standard.
The determination result shows that the novel boron-containing sulphoaluminate cementing material provided by the embodiment meets the requirement of strength grade 42.5.
Example 3
Design C4A 3S% -65%, C2S% -30%, C4 AF% -5%, and M3B%: 0-10 percent, calculating the content of each required raw material, then weighing and proportioning, uniformly mixing and tabletting, wherein the size is phi 30x10 +/-3 mm, and drying in a drying box at 105 ℃.
Placing the prepared raw materials into a crucible, placing the crucible into a high-temperature furnace, calcining the raw materials to perform high-temperature solid-phase reaction, wherein the optimal reaction temperature is as follows: the optimal heat preservation time is as follows at 1300 ℃: and (5) 50 min.
After the high-temperature solid-phase sintering process is finished, the clinker is taken out, air-cooled and quenched to normal temperature, one-step and two-step crushing is carried out, then a proper amount of gypsum is weighed according to the mass percentage of clinker to gypsum of 90: 10, and the mixture is placed in a horizontal ball mill for cement preparation.
And testing the mechanical properties of the prepared cement according to the standard.
The determination result shows that the novel boron-containing sulphoaluminate cementing material provided by the embodiment meets the requirement of strength grade 42.5.
The prepared boron-containing novel sulphoaluminate cementing material is subjected to mechanical property test, and the result is as follows:
| test specimen | 3d | 7d | 28d |
| Example 1 | 28.62MPa | 41.67MPa | 45.99MPa |
| Example 2 | 33.35MPa | 41.26MPa | 47.97MPa |
| Example 3 | 37.82MPa | 42.48MPa | 52.07MPa |
The prepared boron-containing novel sulphoaluminate cementing material is subjected to a radiation protection performance test, and the result is as follows:
| test specimen | M3B 0％ | M3B 2.5％ | M3B 5％ | M3B 7.5％ | M3B 10％ |
| Example 1 | 1.6％ | 6.5％ | 12.3％ | 16.8％ | 22.3％ |
| Example 2 | 1.7％ | 6.6％ | 12.7％ | 16.9％ | 22.4％ |
| Example 3 | 1.7％ | 6.8％ | 12.8％ | 17.0％ | 22.5％ |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A preparation method of a novel boron-containing sulphoaluminate cementing material and a radiation-proof cementing material obtained by the preparation method are characterized by comprising the following steps: in a sulphoaluminate cement raw material system, a boron-containing compound is introduced according to a calculated proportion, a high-temperature solid-phase sintering method is utilized to introduce boron into a mineral phase system, and then the prepared clinker and a proper amount of gypsum are mixed and ground to a certain fineness, so that the novel sulphoaluminate cementing material containing boron is obtained.
2. The preparation method of the boron-containing novel sulphoaluminate cementing material and the obtained radiation-proof cementing material according to the claim 1 are characterized in that: limestone, low-grade bauxite and other raw materials are utilized, ingredients are calculated through a mineral phase content proportioning formula, and the boron-containing sulphoaluminate cement clinker is prepared through solid phase sintering under the high temperature condition.
3. The preparation method of the boron-containing novel sulphoaluminate cementing material and the obtained radiation-proof cementing material according to the claim 1 are characterized in that: the high-temperature solid-phase sintering temperature is 1300-1350 ℃, and the heat-preservation solid-phase reaction time in the sintering process is 20-50 min.
4. The preparation method of the boron-containing novel sulphoaluminate gelled material and the radiation-proof gelled material obtained by the preparation method according to claim 1 are characterized in that: immediately quenching the clinker to normal temperature by adopting an air cooling mode after the high-temperature solid-phase sintering reaction is finished, primarily crushing the clinker to the particle size of 2-10mm, further crushing the clinker to the particle size of less than 1mm by adopting a crusher, adding a proper amount of gypsum, and grinding the mixture by using a ball mill until the residue on the sieve with the particle size of 45 mu m is less than 25%.
5. The preparation method of the boron-containing novel sulphoaluminate cementing material and the obtained radiation-proof cementing material according to the claim 1 are characterized in that: the content range of the boron-containing mineral phase is 0-10%. The clinker comprises the following components in percentage by mass: CaO%: 40-50%, Al2O 3%: 23-33%, SiO 2%: 9-17%, SO 3%: 5-9%, MgO%: 1-7%, B2O 3%: 0.9 to 4 percent.
6. The preparation method of the boron-containing novel sulphoaluminate cementing material and the obtained radiation-proof cementing material according to the claim 1 are characterized in that: the aluminum correction material is mainly one or a mixture of more of alumina, bauxite, kaolin and fly ash.
7. The preparation method of the boron-containing novel sulphoaluminate cementing material and the obtained radiation-proof cementing material according to the claim 1 are characterized in that: the sulfur correcting material is mainly one or a mixture of more of natural gypsum, desulfurized gypsum and phosphogypsum.
8. The preparation method of the boron-containing novel sulphoaluminate cementing material and the obtained radiation-proof cementing material according to the claim 1 are characterized in that: the boron-containing compound is one or a mixture of more of borax, boric anhydride, boron magnesium stone and other raw materials.
9. A radiation protection cement produced by the method for preparing a novel boron-containing sulphoaluminate cement according to any one of claims 1 to 8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011645637.8A CN114685070A (en) | 2020-12-29 | 2020-12-29 | Preparation method of novel boron-containing sulphoaluminate cementing material and radiation-proof cementing material obtained by preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011645637.8A CN114685070A (en) | 2020-12-29 | 2020-12-29 | Preparation method of novel boron-containing sulphoaluminate cementing material and radiation-proof cementing material obtained by preparation method |
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| CN114685070A true CN114685070A (en) | 2022-07-01 |
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