CN106542752A - A kind of native polywater mud material and preparation method thereof - Google Patents
A kind of native polywater mud material and preparation method thereof Download PDFInfo
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- CN106542752A CN106542752A CN201610912315.2A CN201610912315A CN106542752A CN 106542752 A CN106542752 A CN 106542752A CN 201610912315 A CN201610912315 A CN 201610912315A CN 106542752 A CN106542752 A CN 106542752A
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- diaspore
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- polywater mud
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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
- C04B7/00—Hydraulic cements
- C04B7/14—Cements containing slag
- C04B7/147—Metallurgical slag
- C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
- C04B7/1535—Mixtures thereof with other inorganic cementitious materials or other activators with alkali metal containing activators, e.g. sodium hydroxide or waterglass
-
- 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
-
- 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
Abstract
The invention provides a kind of native polywater mud material and preparation method thereof, including following raw material：Diaspore, staurolite, slag, soak, template, sodium hydroxide solution and Cooperative Excitation agent；First, diaspore first passes through soak immersion, and taking out the diaspore after immersion carries out roasting；Then, the diaspore after roasting is carried out into dissolution by Bayer process using template, obtains modified aluminas；Finally, modified aluminas, staurolite and slag are added in the aqueous slkali that sodium hydroxide solution and Cooperative Excitation agent are mixed, stirring reaction, the reaction product for obtaining is native polywater mud material.The present invention makes in diaspore some that hot part solution reaction occur containing aluminosilicate, and generation can be dissolved in the amorphous silica of tert-butylamine pre-polymer solution at a certain temperature, so as to reach desiliconization, purpose so as to improving the utilization ratio of diaspore.
Description
Technical field
The invention belongs to road engineering material field, is related to native polywater mud material, and in particular to a kind of native polywater mud material
And preparation method thereof.
Background technology
Soil polywater mud becomes a pith of Material Field by its premium properties at present.External existing packed soil gathers
Finished cement starts to sell, construction party also gradually start this high performance material has been favored；And China's soil polywater mud
Research applies still at an early stage, and cement of the unit in charge of construction used in work progress mostly is portland cement.Although silicic acid
Ten parts of the application of salt cement extensively, but exists in itself and prepares that energy input is big, environmental pollution is serious etc. and be difficult to
The defect for overcoming, is disagreed with " sustainable development " theory of China, and portland cement will be subject to larger in the use of China
Limit, and performance of the native polywater mud in terms of energy-conserving and environment-protective is significantly better than portland cement, increase the research to native polywater mud
Dynamics is more beneficial for China's green ecological, environment and expanding economy.
China scientific research personnel has been for the research and development of native polywater mud and application to have carried out studying and achieving certain achievement, but
Native polywater mud studies the mainly material based on kaolinite ore and flyash, and the raw material for preparing native polywater mud is slightly single, no
Beneficial to native polywater mud China utilization and extention, therefore it is new for raw material to be badly in need of a kind of non-kaolinite ore of research and development, flyash
Native polywater mud promotes this energy-conserving and environment-protective cement in the application of China widening the raw material field of native polywater mud.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the present invention to provide a kind of native polywater mud material and its preparation
Method, solves the problems, such as that the poly- cement raw material of China's soil is single, promotes energy-conserving and environment-protective cement in the popularization and application of China.
In order to solve above-mentioned technical problem, the present invention is adopted the following technical scheme that and is achieved：
A kind of native polywater mud material, including following raw material makes：Diaspore, staurolite, slag, soak, structure
Template, sodium hydroxide solution and Cooperative Excitation agent；
First, diaspore first passes through soak immersion, and taking out the diaspore after immersion carries out roasting；Then,
Diaspore after roasting is carried out into dissolution by Bayer process using template, modified aluminas are obtained；Finally, will change
Property aluminium oxide, staurolite and slag be added in the aqueous slkali that sodium hydroxide solution and Cooperative Excitation agent are mixed, stirring is anti-
Should, the reaction product for obtaining is native polywater mud material；
Described soak is tert-butylamine pre-polymer solution；
Described template is sodium silicate solution；
Described Cooperative Excitation agent is tert-butylamine pre-polymer solution.
The present invention also has following distinguishing feature：
Described tert-butylamine prepolymer is obtained by procedure below by the tert-butyl alcohol and carbamide：First, carbamide is added, uses matter
Amount concentration is that 30% sulfuric acid solution adjusts pH=7, is 1 in molar ratio by carbamide and tert-butylamine：1 ratio is added, according to urine
Mol ratio between element and the tert-butyl alcohol is 2：1 adds the tert-butyl alcohol, is heated to 45 DEG C, and after being incubated 15 minutes, addition mass concentration is
98% concentrated sulphuric acid, is 2 according to the mol ratio between the concentrated sulphuric acid that carbamide and mass concentration are 98%：1 addition mass concentration be
98% concentrated sulphuric acid, stirs 20 minutes, is subsequently adding the sodium hydroxide solution that mass concentration is 40%, adjusts the pH of reaction system
=9～10, after stirring 10 minutes, observing response system, when there is white haze to produce, the pH=8 in regulation system, naturally cold immediately
But to room temperature, that is, obtain tert-butylamine prepolymer.
The mass concentration of described sodium silicate solution is 50%.
The mass concentration of described sodium hydroxide solution is 40%.
In terms of parts by weight, it is made up of following raw material：Diaspore is 100 parts, and staurolite is 20～80 parts, and slag is
20～80 parts, soak is 95～140 parts, template is 4～10 parts, and sodium hydroxide solution is 4～10 parts, and collaboration swashs
It is 5～10 parts to send out agent.
Preferably, in terms of parts by weight, it is made up of following raw material：Diaspore is 100 parts, and staurolite is 40 parts, ore deposit
Slag is 40 parts, and soak is 120 parts, and template is 7 parts, and sodium hydroxide solution is 7 parts, and Cooperative Excitation agent is 10 parts.
A kind of preparation method of native polywater mud material as above, comprises the following steps：
Step one, diaspore is soaked 24 hours in soak；
The diaspore soaked through step one is carried out roasting by step 2, the roasting at a high temperature of temperature is for 400 DEG C
40 minutes；
Step 3, template is added in the diaspore after step 2 roasting, is existed with Bayer process
Temperature is the dissolution carried out at a temperature of 220 DEG C, obtains modified aluminas；
Step 4, Cooperative Excitation agent and sodium hydroxide solution are mixed and made into into aqueous slkali；
Step 5, modified aluminas, staurolite, slag obtained in step 3 are added separately to into alkali soluble obtained in step 4
In liquid, stir in cement mixer, react 2 hours, the reaction product for obtaining is native polywater mud material.
The present invention compared with prior art, has the following technical effect that：
(I) present invention efficiently make use of diaspore, through the diaspore of tert-butylamine pre-polymer solution immersion,
After using Bayer process roasting certain hour, in making diaspore there is hot part solution reaction containing aluminosilicate in some, generate one
Determine at temperature, to be dissolved in the amorphous silica of tert-butylamine pre-polymer solution, so as to reach desiliconization, purpose so as to improving
The utilization ratio of diaspore.
(II) diaspore soaked through tert-butylamine prepolymer in the present invention, reduces the destruction of aluminium oxide so that
Obtained native polywater mud impurity is less, finer and smoother, intensity is higher.Diaspore is soaked with tert-butylamine so that a hydraulic aluminum
The temperature of stone dissolution aluminium oxide is significantly reduced, and reduces the consumption of the energy.
(III) tert-butylamine pre-polymer solution, sodium hydroxide solution are carried out compounding prepared alkali-activator by the present invention, are excited
Excellent result, and improve the early strength of native polywater mud.
(IV) the obtained soil polywater mud of the present invention has good pavement performance, slag is reused, is promoted
The sustainable development of China's energy, and preparation process is simple of the present invention, low cost, with good economic benefit, are suitable to push away
It is wide to apply.
Explanation is further explained in detail to the particular content of the present invention with reference to embodiments.
Specific embodiment
The specific embodiment of the present invention given below, implement it should be noted that is the invention is not limited in detail below
Example, all equivalents done on the basis of technical scheme each fall within protection scope of the present invention.
Embodiment 1：
The present embodiment provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 20 parts, and slag is 80 parts, and soak is 95 parts, and template is 4 parts, and sodium hydroxide solution is 4 parts,
Cooperative Excitation agent is 5 parts.Wherein：
Soak is tert-butylamine pre-polymer solution, and template is sodium silicate solution, and Cooperative Excitation agent is that tert-butylamine is pre-
Copolymer solution.
Tert-butylamine prepolymer is obtained by procedure below by the tert-butyl alcohol and carbamide：First, carbamide is added, uses mass concentration
Sulfuric acid solution for 30% adjusts pH=7, is 1 in molar ratio by carbamide and tert-butylamine：1 ratio is added, according to carbamide and uncle
Mol ratio between butanol is 2：1 adds the tert-butyl alcohol, is heated to 45 DEG C, after being incubated 15 minutes, adds mass concentration to be 98%
Concentrated sulphuric acid, is 2 according to the mol ratio between the concentrated sulphuric acid that carbamide and mass concentration are 98%：1 adds mass concentration to be 98%
Concentrated sulphuric acid, stirs 20 minutes, is subsequently adding the sodium hydroxide solution that mass concentration is 40%, adjust the pH=9 of reaction system～
10, after stirring 10 minutes, observing response system, when there is white haze to produce, the pH=8 in regulation system, naturally cools to immediately
Room temperature, that is, obtain tert-butylamine prepolymer.
The mass concentration of sodium silicate solution is 50%, and the mass concentration of sodium hydroxide solution is 40%.
The main component of slag includes aluminium oxide, silicon oxide, manganese oxide, and it is 42% left that the content of silicon oxide accounts for total content
The content of the right side, aluminium oxide and silicon oxide accounts for the 80% of total content, and manganese oxide accounts for 10%.
The duct of the modified aluminas that the present embodiment is obtained is in vermiform, and pore size about 7mm to 10mm, quickening react
Speed, improves intensity.
The preparation method of the native polywater mud material of the present embodiment, comprises the following steps：
Step one, diaspore is soaked 24 hours in soak；
The diaspore soaked through step one is carried out roasting by step 2, the roasting at a high temperature of temperature is for 400 DEG C
40 minutes；
Step 3, template is added in the diaspore after step 2 roasting, is existed with Bayer process
Temperature is the dissolution carried out at a temperature of 220 DEG C, obtains modified aluminas；
Cooperative Excitation agent and sodium hydroxide solution are mixed and made into aqueous slkali by step 4；
Modified aluminas, staurolite, slag obtained in step 3 are added separately to alkali soluble obtained in step 4 by step 5
In liquid, stir in cement mixer, react 2 hours, the reaction product for obtaining is native polywater mud material.
Performance test：
Native polywater mud material is poured in three gang moulds, is vibrated 5～10 minutes, is then sealed with polyethylene film, finally existed
Conserve 3～7 days at 60 DEG C, stripping forming.The performance test results are as shown in table 1.
Embodiment 2：
The present embodiment provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 80 parts, and slag is 20 parts, and soak is 140 parts, and template is 10 parts, and sodium hydroxide solution is 10
Part, Cooperative Excitation agent is 10 parts.
In the present embodiment, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is same as Example 1.
The performance test methods of the present embodiment are same as Example 1, and the performance test results are as shown in table 1.
Embodiment 3：
The present embodiment provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 60 parts, and slag is 60 parts, and soak is 120 parts, and template is 7 parts, and sodium hydroxide solution is 7
Part, Cooperative Excitation agent is 10 parts.
In the present embodiment, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is same as Example 1.
The performance test methods of the present embodiment are same as Example 1, and the performance test results are as shown in table 1.
Embodiment 4：
The present embodiment provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 20 parts, and slag is 60 parts, and soak is 110 parts, and template is 6 parts, and sodium hydroxide solution is 6
Part, Cooperative Excitation agent is 10 parts.
In the present embodiment, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is same as Example 1.
The performance test methods of the present embodiment are same as Example 1, and the performance test results are as shown in table 1.
Embodiment 5：
The present embodiment provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 60 parts, and slag is 20 parts, and soak is 130 parts, and template is 9 parts, and sodium hydroxide solution is 8
Part, Cooperative Excitation agent is 10 parts.
In the present embodiment, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is same as Example 1.
The performance test methods of the present embodiment are same as Example 1, and the performance test results are as shown in table 1.
Embodiment 6：
The present embodiment provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 40 parts, and slag is 40 parts, and soak is 120 parts, and template is 7 parts, and sodium hydroxide solution is 7
Part, Cooperative Excitation agent is 10 parts.
In the present embodiment, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is same as Example 1.
The performance test methods of the present embodiment are same as Example 1, and the performance test results are as shown in table 1.
Comparative example 1：(contrasting with embodiment 6, lack soak and Cooperative Excitation agent)
This comparative example provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 40 parts, and slag is 40 parts, and template is 7 parts, and sodium hydroxide solution is 7 parts.
In this comparative example, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is as described below：
Diaspore is carried out roasting by step one, the roasting 40 minutes at a high temperature of temperature is for 400 DEG C；
Step 2, template is added in the diaspore after step one roasting, is existed with Bayer process
Temperature is the dissolution carried out at a temperature of 220 DEG C, obtains modified aluminas；
Step 3, modified aluminas, staurolite, slag obtained in step 2 are added separately in sodium hydroxide solution,
Stir in cement mixer, react 2 hours, the reaction product for obtaining is native polywater mud material.
The performance test methods of this comparative example are same as Example 1, and the performance test results are as shown in table 1.
Comparative example 2：(contrasting with embodiment 6, only lack soak)
This comparative example provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 40 parts, and slag is 40 parts, and template is 7 parts, and sodium hydroxide solution is 7 parts, and Cooperative Excitation agent is
10 parts.
In this comparative example, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is as described below：
Diaspore is carried out roasting by step one, the roasting 40 minutes at a high temperature of temperature is for 400 DEG C；
Step 2, template is added in the diaspore after step one roasting, is existed with Bayer process
Temperature is the dissolution carried out at a temperature of 220 DEG C, obtains modified aluminas；
Cooperative Excitation agent and sodium hydroxide solution are mixed and made into aqueous slkali by step 3；
Step 3, modified aluminas, staurolite, slag obtained in step 2 is added separately in aqueous slkali, in cement
Stir in blender, react 2 hours, the reaction product for obtaining is native polywater mud material.
The performance test methods of this comparative example are same as Example 1, and the performance test results are as shown in table 1.
Comparative example 3：(contrasting with embodiment 6, only lack Cooperative Excitation agent)
This comparative example provides a kind of native polywater mud material, in terms of parts by weight, is made up of following raw material：Diaspore is
100 parts, staurolite is 40 parts, and slag is 40 parts, and soak is 120 parts, and template is 7 parts, and sodium hydroxide solution is 7
Part.
In this comparative example, the selection of raw material and specification are same as Example 1.
The preparation method of the native polywater mud material of the present embodiment is as described below：
Step one, diaspore is soaked 24 hours in soak；
The diaspore soaked through step one is carried out roasting by step 2, the roasting at a high temperature of temperature is for 400 DEG C
40 minutes；
Step 3, template is added in the diaspore after step 2 roasting, is existed with Bayer process
Temperature is the dissolution carried out at a temperature of 220 DEG C, obtains modified aluminas；
Step 4, modified aluminas, staurolite, slag obtained in step 3 are added separately in sodium hydroxide solution,
Stir in cement mixer, react 2 hours, the reaction product for obtaining is native polywater mud material.
The performance test methods of this comparative example are same as Example 1, and the performance test results are as shown in table 1.
1 the performance test results of table
As it can be seen from table 1 compare maintenance 3d, 7d after test specimen indices, it can be found that maintenance 3d after test specimen it is strong
Degree can reach more than the 80% of final strength, illustrate that native polywater mud has higher early strength；Compare the examination of embodiment 1～6
The indices of part, it can be found that every intensity index of embodiment 6 is highest, and every intensity compared with other indexs
Index improves 1～4Mpa, illustrates that the proportioning raw materials of embodiment 6 are most rational；Embodiment 6 and comparative example 1,2,3 are compared, can
To find that the indices intensity of comparative example test specimen does not reach the 50% of 6 intensity index of embodiment, illustrate with present invention enforcement
Obtained in the proportioning raw materials and concrete steps of example 6, native poly- cement performance is more superior.
Claims (7)
1. a kind of native polywater mud material, it is characterised in that make including following raw material：Diaspore, staurolite, slag, leaching
Bubble liquid, template, sodium hydroxide solution and Cooperative Excitation agent；
First, diaspore first passes through soak immersion, and taking out the diaspore after immersion carries out roasting；Then, will roasting
Diaspore after burning carries out dissolution by Bayer process using template, obtains modified aluminas；Finally, by modified oxygen
Change aluminum, staurolite and slag to be added in the aqueous slkali that sodium hydroxide solution and Cooperative Excitation agent are mixed, stirring reaction is obtained
The reaction product for arriving is native polywater mud material；
Described soak is tert-butylamine pre-polymer solution；
Described template is sodium silicate solution；
Described Cooperative Excitation agent is tert-butylamine pre-polymer solution.
2. soil polywater mud material as claimed in claim 1, it is characterised in that described tert-butylamine prepolymer be by the tert-butyl alcohol and
Carbamide is obtained by procedure below：First, carbamide is added, pH=7 is adjusted with the sulfuric acid solution that mass concentration is 30%, by carbamide
It is 1 in molar ratio with tert-butylamine：1 ratio is added, and is 2 according to the mol ratio between carbamide and the tert-butyl alcohol：1 adds the tert-butyl alcohol,
45 DEG C are heated to, after being incubated 15 minutes, the concentrated sulphuric acid that mass concentration is 98% is added, are 98% according to carbamide and mass concentration
Mol ratio between concentrated sulphuric acid is 2：1 addition mass concentration is 98% concentrated sulphuric acid, stirs 20 minutes, is subsequently adding mass concentration
For 40% sodium hydroxide solution, pH=9～10 of reaction system are adjusted, after stirring 10 minutes, observing response system is white when having
When mist is produced, the pH=8 in regulation system, naturally cools to room temperature immediately, that is, obtain tert-butylamine prepolymer.
3. soil polywater mud material as claimed in claim 1, it is characterised in that the mass concentration of described sodium silicate solution is
50%.
4. soil polywater mud material as claimed in claim 1, it is characterised in that the mass concentration of described sodium hydroxide solution is
40%.
5. soil polywater mud material as claimed in claim 1, it is characterised in that in terms of parts by weight, be made up of following raw material：One
Diaspore is 100 parts, and staurolite is 20～80 parts, and slag is 20～80 parts, and soak is 95～140 parts, template
For 4～10 parts, sodium hydroxide solution is 4～10 parts, and Cooperative Excitation agent is 5～10 parts.
6. soil polywater mud material as claimed in claim 5, it is characterised in that in terms of parts by weight, be made up of following raw material：One
Diaspore is 100 parts, and staurolite is 40 parts, and slag is 40 parts, and soak is 120 parts, and template is 7 parts, hydroxide
Sodium solution is 7 parts, and Cooperative Excitation agent is 10 parts.
7. a kind of preparation method of the native polywater mud material as described in claim 1 to 6 any claim, it is characterised in that
Comprise the following steps：
Step one, diaspore is soaked 24 hours in soak；
The diaspore soaked through step one is carried out roasting by step 2,40 points of the roasting at a high temperature of temperature is for 400 DEG C
Clock；
Step 3, template is added in the diaspore after step 2 roasting, with Bayer process in temperature
For the dissolution carried out at a temperature of 220 DEG C, modified aluminas are obtained；
Step 4, Cooperative Excitation agent and sodium hydroxide solution are mixed and made into into aqueous slkali；
Step 5, modified aluminas, staurolite, slag obtained in step 3 are added separately to into aqueous slkali obtained in step 4
In, stirring in cement mixer, react 2 hours, the reaction product for obtaining is native polywater mud material.
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| WO2019019577A1 (en) * | 2017-07-24 | 2019-01-31 | 佛山科学技术学院 | Halloysite geopolymeric cement and manufacturing method therefor |
| CN109369047A (en) * | 2018-12-03 | 2019-02-22 | 佛山科学技术学院 | A kind of high morning native polywater mud and preparation method thereof by force |
| CN112745112A (en) * | 2020-12-25 | 2021-05-04 | 东华大学 | Preparation method of high-strength and high-hardness fine-grain alpha-phase alumina ceramic |
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| CN112745112B (en) * | 2020-12-25 | 2022-07-22 | 东华大学 | Preparation method of high-strength and high-hardness fine-grain alpha-phase alumina ceramic |
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| CN106542752B (en) | 2018-08-31 |
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