CN105967197B - A kind of water glass solution containing graphene and preparation method thereof - Google Patents
A kind of water glass solution containing graphene and preparation method thereof Download PDFInfo
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- CN105967197B CN105967197B CN201610302984.8A CN201610302984A CN105967197B CN 105967197 B CN105967197 B CN 105967197B CN 201610302984 A CN201610302984 A CN 201610302984A CN 105967197 B CN105967197 B CN 105967197B
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
- C01B33/325—After-treatment, e.g. purification or stabilisation of solutions, granulation; Dissolution; Obtaining solid silicate, e.g. from a solution by spray-drying, flashing off water or adding a coagulant
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Abstract
The present invention relates to a kind of water glass solutions containing graphene and preparation method thereof, and the water glass solution is by water, R2O·nSiO2It is formed with graphene.Its preparation process is：By solid R2O·nSiO2, graphene oxide water solution, deionized water press solid content mass ratio 20 ~ 45：0.05~12：0 ~ 79 is uniformly mixed；Obtained mixed liquor is placed in closed stirred autoclave and carries out heating pressurized treatments；By the mixed liquor after the completion of reaction, impurity is removed through natural subsidence, and the liquid of free from admixture part is transferred in concentration tank and is concentrated to corresponding Baume degrees at a certain temperature, the water glass solution containing quantitative graphite alkene is made.Water glass solution application prepared by the present invention is more preferable, and hot property, water resistance enhancing, corrosion resistance improve, and extend the service life that waterglass is applied in every field.The method of the present invention is simple for process, efficient, it is easy to accomplish industrialization production and application.
Description
Technical field
The present invention relates to water glass solutions, are specifically a kind of water glass solution containing graphene and preparation method thereof.
Background technology
The purposes of waterglass is very extensive, is related to the fields such as light industry, chemical industry, building materials, metallurgy, building.Waterglass can apply
Brush is in material surface, raising weatherability, it may also be used for reinforces soil, configuration rapid hardening waterproofing agent, configures resistance to acid gel, is acidproof
Mortar and acid-resisting concrete, antiseptic project etc..Though common waterglass has preferable acid resistance, heat resistance and higher bonding
Power, but waterglass cannot use under alkaline environment, therefore alkali resistance and water resistance are poor, and waterglass is made to be applied in every field
When service life reduce.
Graphene has unique structure and an excellent physicochemical properties, and intensity it is high have huge specific surface area and
The characteristics such as density is small, become the hot spot that researcher gets most of the attention.Graphene is applied in water glass solution, makes it scattered equal
It is even, while enhancing heat resistance, the acid resistance of waterglass, water resistance is improved, to enhance waterglass in every field
Service life.In future, the research and development of waterglass material class will be a brand-new direction, it is contemplated that as a kind of energy saving, inexpensive, ring
The high performance material of border friendly, the sustainable development to realize China's materials industry lay the foundation.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of the water glass solution containing graphene, according to the present invention
Water glass solution water proofing property enhancing prepared by method, resistance to acid and alkali, corrosion resistance improve, and simple for process, efficient, environmentally friendly.
To achieve these goals, the invention is realized by the following technical scheme：
A kind of water glass solution containing graphene, contains water, R2O·nSiO2, graphene.
A kind of preparation method of the water glass solution containing graphene, carries out as follows：
（1）By solid R2O·nSiO2, graphene oxide water solution, deionized water mixed by solid content mass ratio, stir
Duration is mixed more than 30 minutes, mixing speed is more than 200r/min, until being uniformly mixed；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by free from admixture part
Liquid is transferred in concentration tank and is concentrated to corresponding Baume degrees at a certain temperature, as the water glass solution containing graphene.
Further, prioritization scheme of the invention is：
Step（1）The solid R2O·nSiO2, graphene oxide water solution, deionized water be by solid content mass ratio
20~45：0.05~12：0 ~ 79 is mixed.
Step（1）The graphene oxide water solution mass concentration is 0.05 ~ 5%, solid R2O·nSiO2To be inorganic non-
Sodium metasilicate, potassium silicate, lithium metasilicate one of which or several in metallic salt.
Step（2）The closed stirred autoclave treatment process is 0.5 ~ 12 h of hydro-thermal reaction at 100 ~ 230 DEG C,
Pressure is controlled in 1-10 atmospheric pressure.
Step（3）The temperature conditionss are 60 ~ 100 DEG C, and the preferred modulus of the water glass solution containing graphene is 2.0
~ 5.0, Baume degrees is 32 ~ 75 ° of B é.
Using the present invention of above-mentioned technical proposal, have the advantage that compared with prior art：
1. water glass solution application is more preferable, good in thermal property, water proofing property enhancing, service life extend.
2. operating procedure of the present invention is simple, efficient, it is easy to accomplish industrialization production and application.
Specific embodiment
The present invention is described in detail by the following examples, but embodiment does not do any type of limit to the present invention
It is fixed.
Embodiment 1：
A kind of preparation method of the water glass solution containing graphene, carries out as follows：
（1）Solid R2O·2SiO2, 5% graphene oxide water solution, deionized water by solid content mass ratio be 20：0.1：
78, take solid R2O·2SiO220 parts of particle, 2 parts of graphene oxide water solution, deionized water 78 are mixed, and stir duration 35
Minute, 220 r/min of mixing speed, until being uniformly mixed；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments, 100 ~
0.5 ~ 12 h of hydro-thermal reaction at 230 DEG C, pressure are controlled in 1-10 atmospheric pressure；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by free from admixture part
Liquid is transferred in concentration tank and is concentrated at 60 DEG C, obtains the water glass solution containing 5% graphene of 32 ° of B é.
Embodiment 2：
A kind of preparation method of the water glass solution containing graphene, carries out as follows：
（1）Solid R2O·2SiO2, 1% graphene oxide water solution, deionized water by solid content mass ratio be 10：1：0,
Take solid R2O·2SiO220 parts of particle, 200 parts of graphene oxide water solution are mixed, stirring duration 35 minutes, mixing speed
250 r/min, until being uniformly mixed；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments, 100 ~
0.5 ~ 12 h of hydro-thermal reaction at 230 DEG C, pressure are controlled in 1-10 atmospheric pressure；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by free from admixture part
Liquid is transferred in concentration tank and is concentrated at 60 DEG C, obtains the water glass solution containing 1% graphene of 35 ° of B é.
Embodiment 3：
A kind of preparation method of the water glass solution containing graphene, carries out as follows：
（1）Solid R2O·2.6SiO2, 4% graphene oxide water solution, deionized water by solid content mass ratio be 22.5：
3：2.5, take solid R2O·2.6SiO222.5 parts of particle, 75 parts of graphene oxide water solution, 2.5 parts of deionized water are mixed,
Duration 40 minutes, 300 r/min of mixing speed is stirred, until being uniformly mixed；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments, 100 ~
0.5 ~ 12 h of hydro-thermal reaction at 230 DEG C, pressure are controlled in 1-10 atmospheric pressure；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by free from admixture part
Liquid is transferred in concentration tank and is concentrated at 65 DEG C, obtains the water glass solution containing 4% graphene of 42 ° of B é.
Embodiment 4：
A kind of preparation method of the water glass solution containing graphene, carries out as follows：
（1）Solid R2O·2.6SiO2, 5% graphene oxide water solution, deionized water by solid content mass ratio be 25：4：
0, take solid R2O·2.6SiO225 parts of particle, 80 parts of graphene oxide water solution are mixed, stirring duration 40 minutes, stirring
310 r/min of speed, until being uniformly mixed；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments, 100 ~
0.5 ~ 12 h of hydro-thermal reaction at 230 DEG C, pressure are controlled in 1-10 atmospheric pressure；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by free from admixture part
Liquid is transferred in concentration tank and is concentrated at 70 DEG C, obtains the water glass solution containing 5% graphene of 50 ° of B é.
Embodiment 5：
A kind of preparation method of the water glass solution containing graphene, carries out as follows：
（1）Solid R2O·3SiO2, 2.4% graphene oxide water solution, deionized water by solid content mass ratio be 5：1：
0, take solid R2O·3SiO230 parts of particle, 250 parts of graphene oxide water solution are mixed, stirring duration 50 minutes, stirring speed
350 r/min are spent, until being uniformly mixed；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments, 100 ~
0.5 ~ 12 h of hydro-thermal reaction at 230 DEG C, pressure are controlled in 1-10 atmospheric pressure；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by free from admixture part
Liquid is transferred in concentration tank and is concentrated at 78 DEG C, obtains the water glass solution containing 2.4% graphene of 55 ° of B é.
Embodiment 6：
A kind of preparation method of the water glass solution containing graphene, carries out as follows：
（1）Solid R2O·4SiO2, 5% graphene oxide water solution, deionized water by solid content mass ratio be 4：1：0,
Take solid R2O·4SiO240 parts of particle, 200 parts of graphene oxide water solution are mixed, stirring duration 55 minutes, mixing speed
400 r/min, until being uniformly mixed；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments, 100 ~
0.5 ~ 12 h of hydro-thermal reaction at 230 DEG C, pressure are controlled in 1-10 atmospheric pressure；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by free from admixture part
Liquid is transferred in concentration tank and is concentrated at 82 DEG C, obtains the water glass solution containing 5% graphene of 60 ° of B é.
It the above is only the preferred embodiment of the present invention, it is noted that although making with reference to preferred embodiment to the present invention
It is described in detail, for those of ordinary skill in the art, several improvement and profit can be carried out to technical scheme
Decorations, but the spirit and scope of technical solution of the present invention is not departed from, these improvements and modifications are also considered as protection scope of the present invention.
Claims (1)
1. a kind of preparation method of the water glass solution containing graphene, the water glass solution contain water, R2O·nSiO2、
Graphene；It is characterised in that it includes following step：
（1）By solid R2O·nSiO2, graphene oxide water solution, deionized water mixed by solid content mass ratio, during stirring
Long to be more than 30 minutes, mixing speed is more than 200r/min, until being uniformly mixed；The solid R2O·nSiO2, graphene oxide
Aqueous solution, deionized water are 20 ~ 45 by solid content mass ratio：0.05~12：0 ~ 79 is mixed；The graphene oxide water
Concentration of polymer solution is 0.05 ~ 5%, solid R2O·nSiO2For in inorganic non-metallic salt sodium metasilicate, potassium silicate, lithium metasilicate its
Middle one or more；
（2）By step（1）Obtained mixed liquor, which is placed in closed stirred autoclave, carries out heating pressurized treatments；It is described closed to stir
Mixing reaction kettle treatment process is, 0.5 ~ 12 h of hydro-thermal reaction at 100 ~ 230 DEG C, and pressure is controlled in 1-10 atmospheric pressure；
（3）Take out step（2）Mixed liquor after the completion of reaction removes impurity through natural subsidence, and by the liquid of free from admixture part
It is transferred in concentration tank, it is 32 ~ 75 ° of B é, the as water containing graphene to be concentrated to Baume degrees at being 60 ~ 100 DEG C in temperature conditionss
Glass solution, modulus are 2.0 ~ 5.0.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665517A (en) * | 2019-02-25 | 2019-04-23 | 河北北方国能科技有限公司 | The preparation method and application of graphene nano material and modified graphene nano material |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107151465B (en) * | 2017-05-31 | 2019-12-31 | 唐山建华科技发展有限责任公司 | Graphene-containing water-based environment-friendly high-corrosion-resistance zinc-rich primer and preparation method thereof |
| CN110204279A (en) * | 2019-06-13 | 2019-09-06 | 安徽省高等级公路工程监理有限公司 | A kind of configuration method of high durability concrete |
| CN110305712B (en) * | 2019-07-16 | 2021-11-12 | 哈尔滨华帆科技发展有限公司 | Layered silicate loaded graphene lubricating oil additive and preparation method thereof |
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| CN101935036A (en) * | 2009-05-26 | 2011-01-05 | 巴莱诺斯清洁能源控股公司 | Individual layer and the stabilising dispersions of multi-layer graphene layer in solution |
| JP2014107013A (en) * | 2012-11-22 | 2014-06-09 | Dow Corning Toray Co Ltd | Silicon-containing composite material |
| CN104259379A (en) * | 2014-09-30 | 2015-01-07 | 济南圣泉集团股份有限公司 | Collapsibility enhancer for sodium silicate-bonded sand |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935036A (en) * | 2009-05-26 | 2011-01-05 | 巴莱诺斯清洁能源控股公司 | Individual layer and the stabilising dispersions of multi-layer graphene layer in solution |
| JP2014107013A (en) * | 2012-11-22 | 2014-06-09 | Dow Corning Toray Co Ltd | Silicon-containing composite material |
| CN104259379A (en) * | 2014-09-30 | 2015-01-07 | 济南圣泉集团股份有限公司 | Collapsibility enhancer for sodium silicate-bonded sand |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665517A (en) * | 2019-02-25 | 2019-04-23 | 河北北方国能科技有限公司 | The preparation method and application of graphene nano material and modified graphene nano material |
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