CN103241983A - Preparation method of graphene oxide modified polycarboxylic acid type water-reducer - Google Patents
Preparation method of graphene oxide modified polycarboxylic acid type water-reducer Download PDFInfo
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Abstract
The invention relates to a preparation method of a graphene oxide modified polycarboxylic acid type water-reducer. A polycarboxylic acid type water-reducer is a novel efficient water-reducer following a naphthalene type water-reducer, a melamine water-reducer and an amino sulfonic acid based water-reducer, but the mechanical property of concrete cannot be obviously improved by adding the polycarboxylic acid type water-reducer. The preparation method comprises the steps of preparing graphene oxide with natural flake graphite, sodium nitrate, concentrated sulfuric acid and potassium permanganate as raw materials; carrying out ultrasonic dispersion on the graphene oxide; and then adding the polycarboxylic acid type water-reducer with a certain proportion to form an intercalation compound of the graphene oxide and the polycarboxylic acid type water-reducer. With the adoption of the modified water-reducer, on the basisthat the existing water-reducing rate is kept, the flexural strength and the compressive strength of a cement-based composite are obviously strengthened, the relevant raw materials are easily obtained, a preparation technology is reasonable, pollution in a preparation process is little, the performance of products is excellent, and the graphene oxide modified polycarboxylic acid type water-reducer is suitable for industrial production.
Description
Technical field
A kind of modified polycarboxylic acid based water reducer of the present invention is specifically related to a kind of preparation method of graphene oxide modified polycarboxylic acid based water reducer.
Background technology
Poly carboxylic acid series water reducer is the new and effective water reducer after naphthalene system, melamine system and amidosulfonic acid based water reducer.Poly carboxylic acid series water reducer is a kind of anionic polymeric surface active agent in itself, generally with sulfonic group and carboxyl as the major function group in the molecular structure, provide space steric effect with the polyoxyethylene segment, constitute complete pectination.It not only has, and volume is low, the water-reducing rate advantages of higher, can also improve concrete hole structure and compaction rate, be widely used in the engineering that highway, railway, bridge etc. have relatively high expectations to quality, be the key of high-performance green concrete development, but the adding of poly carboxylic acid series water reducer can not obviously improve mechanical properties of concrete.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method that can significantly improve the graphene oxide modified polycarboxylic acid based water reducer of mechanical property after the cement solidification.
The technical solution adopted in the present invention is:
1, the preparation method of graphene oxide modified polycarboxylic acid based water reducer is characterized in that:
Realized by following steps:
Step 1: the preoxidation of graphite:
Be that 98% the vitriol oil, 2.5-3.5 mass parts Potassium Persulphate and 2.5-3.5 mass parts Vanadium Pentoxide in FLAKES join in the reactor successively with 20-30 mass parts, massfraction under agitation condition, be warmed up to 80 ℃, gradation under agitation adds 2-5 mass parts natural graphite raw material, be stirred to evenly, kept 6 hours down at 80 ℃, the filtered sample washing is extremely neutral up to solution, drying for standby;
Step 2: the preparation of graphene oxide:
Under condition of ice bath, with Graphite Powder 99 1.5 mass parts and 1 mass parts SODIUMNITRATE, 60 mass parts, massfraction is that 98% the vitriol oil joins in the reactor successively and mixes, stir the potassium permanganate that in 1 hour, adds the 6-10 mass parts down, be no more than under 5 ℃ the condition stirring reaction in temperature 1 hour, temperature is raised to 35-45 ℃ of stirring reaction 20-30 hour, the deionized water that adds the 400-500 mass parts, temperature is raised to 70-80 ℃ of reaction 30 minutes, the deionized water that adds the 200-300 mass parts again, with 30 mass parts, massfraction is that 30% hydrogen peroxide added in 30 minutes, solution becomes glassy yellow by brown, gained solution is down to room temperature and is carried out centrifugation, deionized water wash, be 7 until washings pH, with the ultrasonication of 350W 1 hour, gained solution is the graphite oxide aqueous solution, and the massfraction of control graphite oxide aqueous solution is 0.5%;
Step 3: the preparation of modified polycarboxylic acid based water reducer:
The massfraction that 10 mass parts graphene oxide solution is joined 90 mass parts, effective constituent is in the poly carboxylic acid series water reducer of 20 %, stirs and with ultrasonication 1 hour, obtains the modified polycarboxylic acid based water reducer.
In the step 3, poly carboxylic acid series water reducer is chosen the poly carboxylic acid series water reducer of being produced by the light building materials in Xi'an Engineering Co., Ltd.
The present invention has the following advantages:
The processing condition of graphene oxide provided by the invention are to prepare the graphene oxide of rich oxygen content (oxygen level is greater than 30%) and the mixture that forms with poly carboxylic acid series water reducer thereof, it is graphene oxide modified polycarboxylic acid based water reducer, water reducer after the modification is on the basis that keeps original water-reducing rate, make the bending and compressive strength of cement-base composite material obviously strengthen, the raw material that the present invention relates to is easy to get, and preparation technology is reasonable, and preparation process is polluted few, excellent product performance is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is graphene oxide spectroscopy detection result.
Embodiment
The present invention will be described in detail below in conjunction with embodiment.
The invention provides rich oxygen content the graphene oxide dispersion liquid the preparation method and with poly carboxylic acid series water reducer method of modifying, the principle of modification mainly is that poly carboxylic acid series water reducer and rich oxygen content graphene oxide have formed intercalated compound, keep the original water-reducing property of poly carboxylic acid series water reducer, and can promote the cement-base composite material hydrated product form shape regular microcrystal, make high performance concrete reach and strengthen toughness reinforcing effect, significantly improved the mechanical property after the cement solidification.
The preparation method of the graphene oxide modified polycarboxylic acid based water reducer that the present invention relates to, realized by following steps:
Step 1: the preoxidation of graphite:
Be that 98% the vitriol oil, 2.5-3.5 mass parts Potassium Persulphate and 2.5-3.5 mass parts Vanadium Pentoxide in FLAKES join in the reactor successively with 20-30 mass parts, massfraction under agitation condition, be warmed up to 80 ℃, gradation under agitation adds 2-5 mass parts natural graphite raw material, be stirred to evenly, kept 6 hours down at 80 ℃, the filtered sample washing is extremely neutral up to solution, drying for standby;
Step 2: the preparation of graphene oxide:
Under condition of ice bath, with Graphite Powder 99 1.5 mass parts and 1 mass parts SODIUMNITRATE, 60 mass parts, massfraction is that 98% the vitriol oil joins in the reactor successively and mixes, stir the potassium permanganate that in 1 hour, adds the 6-10 mass parts down, be no more than under 5 ℃ the condition stirring reaction in temperature 1 hour, temperature is raised to 35-45 ℃ of stirring reaction 20-30 hour, the deionized water that adds the 400-500 mass parts, temperature is raised to 70-80 ℃ of reaction 30 minutes, the deionized water that adds the 200-300 mass parts again, with 30 mass parts, massfraction is that 30% hydrogen peroxide added in 30 minutes, solution becomes glassy yellow by brown, gained solution is down to room temperature and is carried out centrifugation, deionized water wash, be 7 until washings pH, with the ultrasonication of 350W 1 hour, gained solution is the graphite oxide aqueous solution, and the graphene oxide oxygen level is greater than 30%, and the massfraction of control graphite oxide aqueous solution is 0.5%;
Step 3: the preparation of modified polycarboxylic acid based water reducer:
The massfraction that 10 mass parts graphene oxide solution is joined 90 mass parts, effective constituent is in the poly carboxylic acid series water reducer of 20 %, stirs and with ultrasonication 1 hour, obtains the modified polycarboxylic acid based water reducer.
In the step 3, poly carboxylic acid series water reducer is chosen the poly carboxylic acid series water reducer of being produced by the light building materials in Xi'an Engineering Co., Ltd.
Embodiment 1:
Step 1: the preoxidation of graphite:
Be that 98% the vitriol oil, 2.5 mass parts Potassium Persulphates and 2.5 mass parts Vanadium Pentoxide in FLAKESs join in the reactor successively with 20 mass parts, massfraction under agitation condition, be warmed up to 80 ℃, gradation under agitation adds 2 mass parts natural graphite raw materials, be stirred to evenly, kept 6 hours down at 80 ℃, the filtered sample washing is extremely neutral up to solution, drying for standby;
Step 2: the preparation of graphene oxide:
Under condition of ice bath, with Graphite Powder 99 1.5 mass parts and 1 mass parts SODIUMNITRATE, 60 mass parts, massfraction is that 98% the vitriol oil joins in the reactor successively and mixes, stir the potassium permanganate that in 1 hour, adds 6 mass parts down, be no more than under 5 ℃ the condition stirring reaction in temperature 1 hour, temperature is raised to 35 ℃ of stirring reactions 20 hours, the deionized water that adds 400 mass parts, temperature is raised to 70 ℃ of reactions 30 minutes, the deionized water that adds 200 mass parts again, with 30 mass parts, massfraction is that 30% hydrogen peroxide added in 30 minutes, solution becomes glassy yellow by brown, gained solution is down to room temperature and is carried out centrifugation, deionized water wash, be 7 until washings pH, with the ultrasonication of 350W 1 hour, gained solution is the graphite oxide aqueous solution, and the massfraction of control graphite oxide aqueous solution is 0.5%;
Step 3: the preparation of modified polycarboxylic acid based water reducer:
The massfraction that 10 mass parts graphene oxide solution is joined 90 mass parts, effective constituent is in the poly carboxylic acid series water reducer of 20 %, stirs and with ultrasonication 1 hour, obtains the modified polycarboxylic acid based water reducer.
In the step 3, poly carboxylic acid series water reducer is chosen the poly carboxylic acid series water reducer of being produced by the light building materials in Xi'an Engineering Co., Ltd.
Embodiment 2:
Step 1: the preoxidation of graphite:
Be that 98% the vitriol oil, 3 mass parts Potassium Persulphates and 3 mass parts Vanadium Pentoxide in FLAKESs join in the reactor successively with 25 mass parts, massfraction under agitation condition, be warmed up to 80 ℃, gradation under agitation adds 4 mass parts natural graphite raw materials, be stirred to evenly, kept 6 hours down at 80 ℃, the filtered sample washing is extremely neutral up to solution, drying for standby;
Step 2: the preparation of graphene oxide:
Under condition of ice bath, with Graphite Powder 99 1.5 mass parts and 1 mass parts SODIUMNITRATE, 60 mass parts, massfraction is that 98% the vitriol oil joins in the reactor successively and mixes, stir the potassium permanganate that in 1 hour, adds 8 mass parts down, be no more than under 5 ℃ the condition stirring reaction in temperature 1 hour, temperature is raised to 40 ℃ of stirring reactions 25 hours, the deionized water that adds 450 mass parts, temperature is raised to 75 ℃ of reactions 30 minutes, the deionized water that adds 250 mass parts again, with 30 mass parts, massfraction is that 30% hydrogen peroxide added in 30 minutes, solution becomes glassy yellow by brown, gained solution is down to room temperature and is carried out centrifugation, deionized water wash, be 7 until washings pH, with the ultrasonication of 350W 1 hour, gained solution is the graphite oxide aqueous solution, and the massfraction of control graphite oxide aqueous solution is 0.5%;
Step 3: the preparation of modified polycarboxylic acid based water reducer:
The massfraction that 10 mass parts graphene oxide solution is joined 90 mass parts, effective constituent is in the poly carboxylic acid series water reducer of 20 %, stirs and with ultrasonication 1 hour, obtains the modified polycarboxylic acid based water reducer.
In the step 3, poly carboxylic acid series water reducer is chosen the poly carboxylic acid series water reducer of being produced by the light building materials in Xi'an Engineering Co., Ltd.
Product performance test of the present invention:
(USA) detected result as shown in Figure 1 for EDS, EDAX for the X-gamma spectrometer.The graphene oxide oxygen level 34.37% of the present invention's preparation.
The concrete application:
Pressure-proof and snap-resistent intensity experiment: the anti-folding, the ultimate compression strength that have detected cement mortar according to GB/T 50080-2002.Standard sand is produced by Xiamen standard sand factory, meets ISO benchmark sand size distribution and moisture content requirement, the renown cement (P.O 42.5R) that cement adopts Shaanxi renown cement limited-liability company to produce.Mortar is to be puddled by 450 gram cement, 1350 gram standard sands and 150 gram water and water reducer to form.Water reducer is respectively poly carboxylic acid series water reducer (the light building materials in Xi'an Engineering Co., Ltd produces, content 20%) and this patent product, the results are shown in Table 1.
It is cited that content of the present invention is not limited to embodiment, and the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (2)
1. the preparation method of graphene oxide modified polycarboxylic acid based water reducer is characterized in that:
Realized by following steps:
Step 1: the preoxidation of graphite:
Be that 98% the vitriol oil, 2.5-3.5 mass parts Potassium Persulphate and 2.5-3.5 mass parts Vanadium Pentoxide in FLAKES join in the reactor successively with 20-30 mass parts, massfraction under agitation condition, be warmed up to 80 ℃, gradation under agitation adds 2-5 mass parts natural graphite raw material, be stirred to evenly, kept 6 hours down at 80 ℃, the filtered sample washing is extremely neutral up to solution, drying for standby;
Step 2: the preparation of graphene oxide:
Under condition of ice bath, with Graphite Powder 99 1.5 mass parts and 1 mass parts SODIUMNITRATE, 60 mass parts, massfraction is that 98% the vitriol oil joins in the reactor successively and mixes, stir the potassium permanganate that in 1 hour, adds the 6-10 mass parts down, be no more than under 5 ℃ the condition stirring reaction in temperature 1 hour, temperature is raised to 35-45 ℃ of stirring reaction 20-30 hour, the deionized water that adds the 400-500 mass parts, temperature is raised to 70-80 ℃ of reaction 30 minutes, the deionized water that adds the 200-300 mass parts again, with 30 mass parts, massfraction is that 30% hydrogen peroxide added in 30 minutes, solution becomes glassy yellow by brown, gained solution is down to room temperature and is carried out centrifugation, deionized water wash, be 7 until washings pH, with the ultrasonication of 350W 1 hour, gained solution is the graphite oxide aqueous solution, and the massfraction of control graphite oxide aqueous solution is 0.5%;
Step 3: the preparation of modified polycarboxylic acid based water reducer:
The massfraction that 10 mass parts graphene oxide solution is joined 90 mass parts, effective constituent is in the poly carboxylic acid series water reducer of 20 %, stirs and with ultrasonication 1 hour, obtains the modified polycarboxylic acid based water reducer.
2. the preparation method of graphene oxide modified polycarboxylic acid based water reducer according to claim 1 is characterized in that:
In the step 3, poly carboxylic acid series water reducer is chosen the poly carboxylic acid series water reducer of being produced by the light building materials in Xi'an Engineering Co., Ltd.
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| RU2783099C2 (en) * | 2021-03-24 | 2022-11-08 | ФЕДЕРАЛЬНОЕ ГОСУДАРСТВЕННОЕ БЮДЖЕТНОЕ УЧРЕЖДЕНИЕ "РОССИЙСКИЙ НАУЧНЫЙ ЦЕНТР РАДИОЛОГИИ И ХИРУРГИЧЕСКИХ ТЕХНОЛОГИЙ ИМЕНИ АКАДЕМИКА А.М. ГРАНОВА" МИНИСТЕРСТВА ЗДРАВООХРАНЕНИЯ РОССИЙСКОЙ ФЕДЕРАЦИИ / ФГБУ "РНЦРХТ им. академика А.М. Гранова" Минздрава России | Method for scaling synthesis of graphene oxide |
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| CN117819864A (en) * | 2024-03-04 | 2024-04-05 | 四川蜀道建筑科技有限公司 | Polycarboxylic acid high-performance water reducer |
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