CN110591838A - Graphene type oil-removing additive and preparation method thereof - Google Patents
Graphene type oil-removing additive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/06—Phosphates, including polyphosphates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/1233—Carbonates, e.g. calcite or dolomite
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/14—Fillers; Abrasives ; Abrasive compositions; Suspending or absorbing agents not provided for in one single group of C11D3/12; Specific features concerning abrasives, e.g. granulometry or mixtures
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
- C11D3/225—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC
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Abstract
The invention discloses a graphene type oil-removing additive and a preparation method thereof, belonging to the technical field of oil stain removal. A preparation method of a graphene type oil-removing additive comprises the following steps: s1, preparing graphene oxide by using a Hummers method; s2, adding water into graphene oxide, performing ultrasonic dispersion to form a graphene oxide dispersion solution, adding L-ascorbic acid, continuing performing ultrasonic treatment for 30-50 min, adding methyl hydroxypropyl cellulose, sodium phosphate and calcium carbonate, and heating to 70-90 ℃ to react for 4-6 h; and S3, after S2 is finished, washing the mixture for 2-3 times by using deionized water, and then carrying out freeze drying to obtain the graphene type oil-removing additive. The content of the additive can slowly seep out in the using process, so that the aims of gradual thickening and gradual increase of friction feeling are fulfilled, and the effect of the oil removing agent is improved.
Description
Technical Field
The invention belongs to the technical field of oil stain removal, and particularly relates to a graphene type oil removal additive and a preparation method thereof.
Background
In the machine maintenance industry, when working, a worker often contacts a machine to be repaired with hands, and the general maintenance parts have engine oil, lubricating oil and the like, so that the hands of the worker are contaminated. In daily life, people can often see that the machine maintenance personnel are stained with the engine oil after completing the operation, the oil stain is difficult to clean by using a common cleaning agent, some cleaning agents are greasy when being washed, and meanwhile, the problems of long cleaning time, low cleaning efficiency and poor cleaning effect exist, and the requirements of the operation personnel cannot be met.
For oil removing products such as oil removing agents, cleaning agents and the like, the selection of additives is very important, and the oil removing and dirt removing effects can be indirectly influenced. According to the invention, graphene is used as a basic raw material, and is subjected to surface modification, so that the graphene is used as an oil removing additive, and has a good auxiliary effect on removing oil stains.
Disclosure of Invention
Based on the existing problems, the invention provides a graphene type oil-removing additive and a preparation method thereof, and the additive has the effects of gradually enhancing thickening feeling and friction feeling and enhancing the effect of cleaning oil stains.
The technical scheme adopted by the invention is as follows:
a preparation method of a graphene type oil-removing additive comprises the following steps:
s1, preparing graphene oxide by using a Hummers method;
s2, adding water into graphene oxide, performing ultrasonic dispersion to form a graphene oxide dispersion solution, adding L-ascorbic acid, continuing performing ultrasonic treatment for 30-50 min, adding methyl hydroxypropyl cellulose, sodium phosphate and calcium carbonate, and heating to 70-90 ℃ to react for 4-6 h;
and S3, after S2 is finished, washing the mixture for 2-3 times by using deionized water, and then carrying out freeze drying to obtain the graphene type oil-removing additive.
Specifically, the Hummers method is as follows: 230mL of concentrated H is measured2SO4Putting the beaker into an ice water bath, and keeping the temperature of the beaker at 0-5 ℃; under the state of slow stirring, 10g of graphite powder and 5g of NaNO are taken3Fully mixing, then slowly adding into a beaker, and stirring for 1h after the adding is finished; continuing to slowly add 30g of KMnO4Stirring in ice water bath for 1h after the addition is finished, then heating to 35 ℃, and stirring for 2 h; then cooled to room temperature, 500mL deionized water was slowly added, and 30% H was added2O2Adding 10mL of the solution until no yellow bubbles appear, wherein the color of the solution is bright yellow; filtering while the solution is hot, and fully washing the solution by using 5 percent hydrochloric acid and deionized water until the solution is added with BaCl2And detecting the filtrate by using the solution until no white precipitate is generated, namely the preparation of the graphene oxide is finished.
Further, the concentration of the graphene oxide dispersion liquid is 2-5 mg/mL.
Further, the mass of the L-ascorbic acid is 1-3 times of that of the graphene oxide.
Further, the mass of the methyl hydroxypropyl cellulose is 1-2 times of that of the graphene.
Further, the sodium phosphate and the calcium carbonate are obtained by ball milling for 10 hours through a ball mill and sieving through a 300-mesh sieve according to the mass ratio of 1: 3; the mass of the sodium phosphate is 0.2-0.5 times of that of the graphene oxide.
Further, the temperature of the freeze-dried cold trap in the S3 is-50 to-60 ℃, and the no-load vacuum degree is 15 to 18 Pa.
A graphene type oil-removing additive prepared by the method of any one of claims 1 to 6.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: the graphene oxide prepared by the Hummers method contains a large number of oxygen-containing functional groups on the surface, has strong hydrophilicity and electrostatic repulsion effect, is damaged after a reducing agent L-ascorbic acid is added for thermal reaction, and the reduction of the oxygen-containing functional groups enables the graphene to recover a conjugated structure again and interact to cause random accumulation among graphene sheet layers, so that a three-dimensional structure is formed; and then adding methyl hydroxypropyl cellulose and unreacted oxygen-containing functional groups for cross-linking reaction to obtain a network three-dimensional porous material, and then adding sodium phosphate and calcium carbonate into the network three-dimensional porous material, so that the sodium phosphate and the calcium carbonate slowly exude in the using process to achieve the purposes of gradual thickening and gradual increase of friction feeling, thereby improving the effect of the oil remover.
Detailed Description
The embodiments of the present invention can be obtained by different substitutions in specific ranges based on the above technical solutions, and therefore, the following embodiments are only preferred embodiments of the embodiments, and any technical substitutions made by the above technical solutions are within the protection scope of the present invention.
Example 1
A preparation method of a graphene type oil-removing additive comprises the following steps:
s1, graphene oxide prepared by Hummers method: 230mL of concentrated H is measured2SO4Placing the beaker into an ice water bath, and keeping the temperature of the beaker at 0 ℃; under the state of slow stirring, 10g of graphite powder and 5g of NaNO are taken3Fully mixing, then slowly adding into a beaker, and stirring for 1h after the adding is finished; continuing to slowly add 30g of KMnO4Stirring in ice water bath for 1h after the addition is finished, then heating to 35 ℃, and stirring for 2 h; then cooled to room temperature, 500mL deionized water was slowly added, and 30% H was added2O2Adding 10mL of the solution until no yellow bubbles appear, wherein the color of the solution is bright yellow; filtering while the solution is hot, and fully washing the solution by using 5 percent hydrochloric acid and deionized water until the solution is added with BaCl2Detecting the filtrate until no white precipitate is generated by the solution detection, namely completing the preparation of the graphene oxide;
s2, adding water into graphene oxide, performing ultrasonic dispersion to form graphene oxide dispersion liquid with the concentration of 2mg/mL, adding L-ascorbic acid with the mass of 1 time that of the graphene oxide, continuing performing ultrasonic treatment for 30min, adding methyl hydroxypropyl cellulose, sodium phosphate and calcium carbonate with the mass of 1 time that of the graphene, and heating to 70 ℃ to react for 4 h; the sodium phosphate and the calcium carbonate are obtained by ball milling for 10h through a ball mill and sieving through a 300-mesh sieve according to the mass ratio of 1: 3; the mass of the sodium phosphate is 0.2 times of that of the graphene oxide;
and S3, after S2 is finished, washing the mixture for 2 times by using deionized water, and then carrying out freeze drying at the cold trap temperature of-50 ℃ and the no-load vacuum degree of 15Pa to obtain the graphene type oil-removing additive.
Example 2
A preparation method of a graphene type oil-removing additive comprises the following steps:
s1, graphene oxide prepared by Hummers method:230mL of concentrated H is measured2SO4Placing the beaker into an ice water bath, and keeping the temperature of the beaker at 2 ℃; under the state of slow stirring, 10g of graphite powder and 5g of NaNO are taken3Fully mixing, then slowly adding into a beaker, and stirring for 1h after the adding is finished; continuing to slowly add 30g of KMnO4Stirring in ice water bath for 1h after the addition is finished, then heating to 35 ℃, and stirring for 2 h; then cooled to room temperature, 500mL deionized water was slowly added, and 30% H was added2O2Adding 10mL of the solution until no yellow bubbles appear, wherein the color of the solution is bright yellow; filtering while the solution is hot, and fully washing the solution by using 5 percent hydrochloric acid and deionized water until the solution is added with BaCl2Detecting the filtrate until no white precipitate is generated by the solution detection, namely completing the preparation of the graphene oxide;
s2, adding water into graphene oxide, performing ultrasonic dispersion to form graphene oxide dispersion liquid with the concentration of 4mg/mL, adding L-ascorbic acid with the mass being 2 times that of the graphene oxide, continuing performing ultrasonic treatment for 40min, adding methyl hydroxypropyl cellulose, sodium phosphate and calcium carbonate with the mass being 1.5 times that of the graphene, and heating to 80 ℃ to react for 5 h; the sodium phosphate and the calcium carbonate are obtained by ball milling for 10h through a ball mill and sieving through a 300-mesh sieve according to the mass ratio of 1: 3; the mass of the sodium phosphate is 0.3 times of that of the graphene oxide;
and S3, after S2 is finished, washing the mixture for 2 times by using deionized water, and then carrying out freeze drying at the cold trap temperature of-55 ℃ and the no-load vacuum degree of 16Pa to obtain the graphene type oil-removing additive.
Example 3
A preparation method of a graphene type oil-removing additive comprises the following steps:
s1, graphene oxide prepared by Hummers method: 230mL of concentrated H is measured2SO4Placing the beaker into an ice water bath, and keeping the temperature of the beaker at 4 ℃; under the state of slow stirring, 10g of graphite powder and 5g of NaNO are taken3Fully mixing, then slowly adding into a beaker, and stirring for 1h after the adding is finished; continuing to slowly add 30g of KMnO4Stirring in ice water bath for 1h after the addition is finished, then heating to 35 ℃, and stirring for 2 h; then cooled to room temperature, 500mL deionized water was slowly added, and 30% H was added2O210mL plusUntil no yellow bubbles appear, the solution is bright yellow; filtering while the solution is hot, and fully washing the solution by using 5 percent hydrochloric acid and deionized water until the solution is added with BaCl2Detecting the filtrate until no white precipitate is generated by the solution detection, namely completing the preparation of the graphene oxide;
s2, adding water into graphene oxide, performing ultrasonic dispersion to form a graphene oxide dispersion liquid with the concentration of 4mg/mL, adding L-ascorbic acid with the mass 1.5 times that of the graphene oxide, continuing performing ultrasonic treatment for 45min, adding methyl hydroxypropyl cellulose, sodium phosphate and calcium carbonate with the mass 1.5 times that of the graphene, and heating to 80 ℃ to react for 4.5 h; the sodium phosphate and the calcium carbonate are obtained by ball milling for 10h through a ball mill and sieving through a 300-mesh sieve according to the mass ratio of 1: 3; the mass of the sodium phosphate is 0.4 times of that of the graphene oxide;
and S3, after S2 is finished, washing the mixture for 2 times by using deionized water, and then carrying out freeze drying at the cold trap temperature of-55 ℃ and the no-load vacuum degree of 18Pa to obtain the graphene type oil-removing additive.
Example 4
A preparation method of a graphene type oil-removing additive comprises the following steps:
s1, graphene oxide prepared by Hummers method: 230mL of concentrated H is measured2SO4Placing the beaker into an ice water bath, and keeping the temperature of the beaker at 5 ℃; under the state of slow stirring, 10g of graphite powder and 5g of NaNO are taken3Fully mixing, then slowly adding into a beaker, and stirring for 1h after the adding is finished; continuing to slowly add 30g of KMnO4Stirring in ice water bath for 1h after the addition is finished, then heating to 35 ℃, and stirring for 2 h; then cooled to room temperature, 500mL deionized water was slowly added, and 30% H was added2O2Adding 10mL of the solution until no yellow bubbles appear, wherein the color of the solution is bright yellow; filtering while the solution is hot, and fully washing the solution by using 5 percent hydrochloric acid and deionized water until the solution is added with BaCl2Detecting the filtrate until no white precipitate is generated by the solution detection, namely completing the preparation of the graphene oxide;
s2, adding water into graphene oxide, performing ultrasonic dispersion to form a graphene oxide dispersion liquid with the concentration of 5mg/mL, adding L-ascorbic acid with the mass being 3 times that of the graphene oxide, continuing performing ultrasonic treatment for 50min, adding methyl hydroxypropyl cellulose, sodium phosphate and calcium carbonate with the mass being 2 times that of the graphene, and heating to 90 ℃ to react for 6 h; the sodium phosphate and the calcium carbonate are obtained by ball milling for 10h through a ball mill and sieving through a 300-mesh sieve according to the mass ratio of 1: 3; the mass of the sodium phosphate is 0.5 times of that of the graphene oxide;
and S3, after S2 is finished, washing the mixture for 3 times by using deionized water, and then carrying out freeze drying at the cold trap temperature of-60 ℃ and the no-load vacuum degree of 18Pa to obtain the graphene type oil-removing additive.
Comparative example 1
The difference from example 1 is that: the concentration of the graphene oxide dispersion was 0.5 mg/mL.
Comparative example 2
The difference from example 1 is that: the reaction temperature in S2 was 50 ℃.
Comparative example 3
The difference from example 1 is that: the mass of the L-ascorbic acid is 0.5 times that of the graphene oxide.
The additives obtained in the above examples and comparative examples were subjected to related performance tests, and an anionic surfactant was compounded with the additive of the present invention, and the thickening and frictional feeling were observed, and the results are shown in table 1 using the anionic surfactant as a reference.
Table 1 results of performance testing
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (7)
1. A preparation method of a graphene type oil-removing additive is characterized by comprising the following steps:
s1, preparing graphene oxide by using a Hummers method;
s2, adding water into graphene oxide, performing ultrasonic dispersion to form a graphene oxide dispersion solution, adding L-ascorbic acid, continuing performing ultrasonic treatment for 30-50 min, adding methyl hydroxypropyl cellulose, sodium phosphate and calcium carbonate, and heating to 70-90 ℃ to react for 4-6 h;
and S3, after S2 is finished, washing the mixture for 2-3 times by using deionized water, and then carrying out freeze drying to obtain the graphene type oil-removing additive.
2. The method of claim 1, wherein the graphene oxide dispersion has a concentration of 2-5 mg/mL.
3. The method of claim 1, wherein the mass of the L-ascorbic acid is 1-3 times of the mass of the graphene oxide.
4. The method of claim 1, wherein the mass of the methylhydroxypropylcellulose is 1-2 times the mass of the graphene.
5. The method for preparing the graphene type oil-removing additive according to claim 1, wherein the sodium phosphate and the calcium carbonate are obtained by ball milling for 10 hours and passing through a 300-mesh sieve in a mass ratio of 1:3 by a ball mill; the mass of the sodium phosphate is 0.2-0.5 times of that of the graphene oxide.
6. The method for preparing the graphene type oil-removing additive according to claim 1, wherein the cold trap temperature of freeze drying in S3 is-50 to-60 ℃, and the no-load vacuum degree is 15 to 18 Pa.
7. A graphene type oil-removing additive characterized by being prepared by the method of any one of claims 1 to 6.
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Application publication date: 20191220 |