A dispersion, a method for producing the same, and use thereof

Abstract

The application discloses a dispersion liquid and a preparation method and application thereof. The dispersion liquid comprises the following components per 100 parts by weight: a polymer dispersant, 10-60 parts; hydrophilic graphene, 0.01-10 parts; a small molecule surfactant, 0.05-10 parts; and water. The dispersion liquid has simple composition, strong and various functions, the amount of the polymer dispersant is greatly reduced (the amount of the polymer dispersant can be reduced by up to 12% under the same dispersion condition), the dispersibility and stability of organic pigments in water can be remarkably improved, and the dispersion liquid is very suitable for selection of the cosmetic industry. The preparation method of the dispersion liquid is simple and clear, and has strong operability.

Description

TECHNICAL FIELD

[0001] The present application relates to a dispersion liquid and a preparation method and application thereof. BACKGROUND

[0002] Cosmetic is a best-selling category of cosmetics, with huge market sales. The manufacture of cosmetic products requires the use of various pigments, such as carbon black, titanium white and various organic pigments, and the use of dispersants to disperse the pigments to form stable color paste.

[0003] The early commonly used pigment dispersants are mainly small molecule surfactants, which are mainly non-ionic ethylene oxide, anionic sulfonate, carboxylate and phosphate, cationic quaternary ammonium salt, quaternary phosphonium salt, etc. They have certain dispersion stability in aqueous solution, but their adsorption with pigment particles is not close, and they are easy to desorb from the surface of the pigment, leading to the re-aggregation of the dispersed pigment particles, resulting in flocculation or precipitation.

[0004] Later, with the development of polymer industry, polymer dispersants became the mainstream choice. The molecular weight of general polymer dispersants is between 1000-30000, and the molecular structure contains two parts of anchoring group and solvation chain. Among them, the anchoring group can be firmly adsorbed on the surface of pigment particles by hydrogen bond, ionic bond, covalent bond, etc. in single adsorption or multi-point anchoring mode, and the common ones are amino, hydroxyl, carboxyl, sulfonic acid group, phosphoric acid group, ether bond, etc. The solvation chain generally refers to flexible alkyl chain, which can form a certain thickness of protective layer on the surface of solid particles, and plays a stabilizing role in the dispersion of particles through steric hindrance. However, the current use amount of polymer dispersant is high, which leads to the increase of cost, and also affects the quality of cosmetics, causing safety hazards to the use and physical and mental health of consumers. Therefore, how to use a small amount of dispersant to prepare stable pigment slurry in the pigment dispersion process is a challenge problem in this field. In addition, giving the dispersant other functions besides dispersion and diversifying its functions are also the development direction of the field in the future. SUMMARY

[0005] The technical problem solved by the present application is to provide a dispersion liquid and a preparation method and application thereof in order to overcome the defects of high use amount of polymer dispersant, high cost and single function in the prior art. The dispersion liquid has simple composition, powerful and diverse functions, and the use amount of polymer dispersant in it is greatly reduced (up to 12% under the same dispersion conditions), which can significantly improve the dispersibility and stability of organic pigments in water, and is very suitable for selection in the cosmetic industry. The preparation method of the dispersion liquid is simple and easy to operate.

[0006] The graphene molecules are very easy to agglomerate and are not conducive to dispersion, and the functional effects of graphene materials and dispersants are greatly different, and currently, there is no research on using graphene to prepare a dispersion liquid in the prior art. In the present application, the applicant has found through a large number of experimental researches that a large number of hydrophilic groups on the surface of hydrophilic graphene can help the organic pigment wrapped by the graphene to be stably dispersed in water, and the prepared dispersion liquid has simple composition, powerful and diverse functions, the amount of the polymer dispersant is greatly reduced, the dispersibility and stability of the organic pigment in water can be significantly improved, and the dispersion liquid is very suitable for selection of the cosmetic industry.

[0007] The present application solves the above technical problems through the following technical solutions.

[0008] The present application provides a dispersion liquid, which comprises the following components per 100 parts by weight:

[0009] Polymer dispersant: 10-60 parts;

[0010] Hydrophilic graphene: 0.01-10 parts;

[0011] Small molecule surfactant: 0.05-10 parts;

[0012] And water.

[0013] In the present application, the hydrophilic graphene can be various forms of hydrophilic graphene materials that can be dispersed in water in the art, preferably one or more of graphene oxide, sulfonated graphene, carboxylated graphene and PEGylated graphene, and more preferably graphene oxide.

[0014] Those skilled in the art can understand that the PEGylated graphene in the present application is a product obtained by chemical reaction of polyethylene glycol and graphene.

[0015] In the present application, the amount of the hydrophilic graphene is preferably 0.05-1 parts per 100 parts by weight of the dispersion liquid, more preferably 0.05-0.25 parts, for example 0.1 parts.

[0016] In the present application, the molecular weight of the polymer dispersant does not need to be particularly controlled, and those skilled in the art can select according to actual needs, for example, selecting a polymer dispersant with a molecular weight of 1000-10000, preferably a polymer dispersant with a molecular weight of 2000-5000, more preferably a polymer dispersant with a molecular weight of 2000-3000, a polymer dispersant with a molecular weight of 3000-4000, or a polymer dispersant with a molecular weight of 3000-5000.

[0017] In the present application, the polymer dispersant can be one or more of styrene-acrylate copolymer, styrene-maleic anhydride copolymer, polyvinylpyrrolidone, polyacrylamide-acrylic acid copolymer, acrylate polymer, nonylphenol polyoxyethylene ether, sodium fatty alcohol polyoxyethylene ether sulfate and polyurethane, preferably styrene-acrylate copolymer and / or acrylate polymer, more preferably styrene-methyl methacrylate copolymer and / or acrylate polymer, such as styrene-methyl methacrylate-acrylic acid polymer, methyl methacrylate-methacrylic acid polymer or acrylic resin polymer.

[0018] Preferably, the molecular weight of the styrene-methyl methacrylate-acrylic acid polymer is 3000-5000.

[0019] Preferably, the method and conditions for preparing the styrene-methyl methacrylate-acrylic acid polymer are conventional in the art.

[0020] Preferably, the molar ratio of styrene, methyl methacrylate and acrylic acid contained in the styrene-methyl methacrylate-acrylic acid polymer is 1:1:1.

[0021] Preferably, the molecular weight of the methyl methacrylate-methacrylic acid polymer is 3000-4000.

[0022] Preferably, the method and conditions for preparing the methyl methacrylate-methacrylic acid polymer are conventional in the art.

[0023] Preferably, the molar ratio of methyl methacrylate and methacrylic acid contained in the methyl methacrylate-methacrylic acid polymer is 1:1.

[0024] Preferably, the molecular weight of the acrylic resin polymer is 2000-3000.

[0025] Preferably, the acrylic resin polymer is acrylic resin polymer of type J678 from BASF.

[0026] In the present application, the amount of the polymer dispersant is preferably 25-35 parts per 100 parts by weight of the dispersion, more preferably 33.3 parts.

[0027] In the present application, the molecular weight of the small molecule surfactant is usually below 1000.

[0028] As understood by those skilled in the art, the small molecule surfactant in the present application refers to small molecule surfactants with definite chemical structural formula, such as quaternary ammonium salt, quaternary phosphonium salt or sulfonate.

[0029] In the present application, the small molecule surfactant can be a small molecule anionic surfactant and / or a small molecule nonionic surfactant. The small molecule anionic surfactant can be one or more of sodium alkyl benzene sulfonate, sodium lauryl sulfate and lauroyl glutamic acid, preferably sodium lauryl sulfate. The small molecule nonionic surfactant can be glyceryl stearate and / or fatty acid glyceride.

[0030] In the present application, the amount of the small molecule surfactant is preferably 0.05-0.5 parts, for example 0.3 parts, per 100 parts by weight of the dispersion.

[0031] In the present application, the amount of water can be selected according to actual needs. The amount of water can be 50-60 parts, preferably 55-58 parts, for example 57.15 parts, 57.3 parts or 57.35 parts, per 100 parts by weight of the dispersion.

[0032] In the present application, the dispersion preferably further comprises an auxiliary.

[0033] The specific type and amount of the auxiliary can be selected according to actual needs.

[0034] The type of the auxiliary can be conventional in the art, for example one or more of a preservative, a humectant and a wetting agent, preferably a preservative and a humectant.

[0035] The amount of the auxiliary can be 0-20 parts, preferably 0-15 parts, for example 0.1-8 parts, per 100 parts by weight of the dispersion.

[0036] When the auxiliary comprises a preservative, the preservative can be one or more of an aromatic alcohol, an aromatic acid, a fatty alcohol and an aldehyde substance, for example one or more of benzyl alcohol, phenoxyethanol, benzoic acid, salicylic acid and sorbic acid.

[0037] When the auxiliary comprises a preservative, the amount of the preservative can be 0-5 parts, but not 0 parts, per 100 parts by weight of the dispersion, preferably 0.1-2 parts, for example 1 part.

[0038] When the auxiliary comprises a humectant, the humectant can be one or more of a polyhydric alcohol, a sugar and a natural plant extract, preferably a polyhydric alcohol, more preferably one or more of glycerol, butylene glycol, polyethylene glycol, propylene glycol, hexylene glycol, xylitol and sorbitol, for example propylene glycol or butylene glycol.

[0039] When the humectant comprises a sugar, the sugar can be one or more of trehalose, sodium hyaluronate and methyl gluceth.

[0040] When the humectant includes a natural extract, the natural extract can be a conventional natural extract in the art.

[0041] When the auxiliary agent includes a humectant, the humectant can be used in an amount of 0-15 parts per 100 parts by weight of the dispersion, but not 0 parts, preferably 4-10 parts, for example 6 parts or 8 parts.

[0042] When the auxiliary agent includes a wetting agent, the wetting agent can be one or more of sulfonated oil, soybean lecithin, mercaptans, hydrazides and organosilicon substances, for example organosilicon substances.

[0043] In the present application, preferably, 100 parts by weight of the dispersion includes: 25-35 parts of a polymeric dispersant, 0.05-0.25 parts of graphene oxide, 0.05-0.5 parts of a small-molecule anionic surfactant, and water,

[0044] More preferably, 100 parts by weight of the dispersion includes: 25-35 parts of a polymeric dispersant, 0.05-0.25 parts of graphene oxide, 0.05-0.5 parts of a small-molecule anionic surfactant, 0.1-2 parts of a preservative, 4-10 parts of a humectant, and 50-60 parts of water.

[0045] For example, 100 parts by weight of the dispersion includes: 33.3 parts of a styrene-methyl methacrylate-acrylic acid copolymer with a molecular weight of 3000-5000, 0.1 parts of graphene oxide, 0.3 parts of sodium lauryl sulfate, 1 part of phenoxyethanol, and 8 parts of butanediol, and the balance is water.

[0046] The present application also provides a preparation method of the dispersion as described above, which includes the following preparation steps: uniformly mixing the components in the dispersion.

[0047] In the present application, the source of the hydrophilic graphene can be commercially available or prepared by conventional methods in the art.

[0048] When the hydrophilic graphene is prepared, the preparation method thereof preferably includes the following steps:

[0049] The solution containing the hydrophilic graphite raw material is subjected to several times of "peeling, centrifugation and separation" to obtain a supernatant, and the solvent in the supernatant is removed, and then dried.

[0050] The hydrophilic graphite raw material can be sulfonated graphite and / or graphene oxide, preferably graphene oxide.

[0051] The peeling method can be one or more of stirring, ultrasonic and shearing, preferably stirring and ultrasonic. The stirring rate can be conventional in the art. The stirring time can be conventional in the art, for example 30 min. The ultrasonic time can be conventional in the art, for example 20 min.

[0052] The centrifugal device can be conventional in the art, for example a high-speed centrifuge. The high-speed centrifuge can rotate at a speed of 5000-20000 rpm, preferably 12000 rpm.

[0053] The pH value of the supernatant can be conventional in the art for preparing hydrophilic graphene, preferably 6-7.

[0054] The method for removing the solvent in the supernatant can be conventional in the art, preferably reduced pressure distillation.

[0055] The solvent can be conventional in the art, for example one or more of deionized water, anhydrous ethanol and propanol, preferably deionized water.

[0056] The drying method can be conventional in the art, for example vacuum drying.

[0057] In the present application, the mixing device can be conventional in the art, for example a homogenizer. The stirring speed of the homogenizer can be 1000-15000 rpm, preferably 10000-13000 rpm. The stirring time of the homogenizer can be 0.5-5 hours, preferably 2-3 hours, for example 2.5 hours. The stirring temperature of the homogenizer can be 0-50°C, preferably 20-30°C, for example 25°C. The stirring speed, temperature and time of the homogenizer are interdependent, and ultimately make the dispersion stable.

[0058] In a preferred embodiment of the present application, the preparation method of the dispersion is provided as follows:

[0059] Step (1): Preparation of hydrophilic graphene material

[0060] Deionized water is added to the hydrophilic graphite raw material, which is peeled into a hydrophilic graphene slurry crude product dispersed in water by mechanical stirring, ultrasonic or shearing, and then high-speed centrifugal separation is performed at 5000-20000 rpm. The obtained precipitate is repeatedly subjected to the above-mentioned water dispersion, peeling and centrifugal process until the pH value of the supernatant is 6-7. All the supernatants after centrifugation are collected, the solvent is evaporated under reduced pressure, and then vacuum drying is performed to obtain a hydrophilic graphene powder material.

[0061] Step (2): Preparation of dispersion

[0062] The polymer dispersant, hydrophilic graphene, small molecule surfactant, preservative and deionized water are mixed together according to the weight ratio, and are uniformly mixed by using a homogenizer to obtain.

[0063] In step (1), the raw material of the hydrophilic graphite is selected from sulfonated graphite and / or oxidized graphite, preferably oxidized graphite.

[0064] In step (2), the stirring speed of the homogenizer is 1000-15000 rpm, preferably 10000-13000 rpm. The stirring time of the homogenizer is 0.5-5 hours, preferably 2-3 hours, for example 2.5 hours. The stirring temperature of the homogenizer is 0-50℃, preferably 20-30℃, for example 25℃.

[0065] The present application also provides the use of the dispersion liquid as described above in the cosmetic industry.

[0066] In the present application, the dispersion liquid can be used to disperse common raw materials used in cosmetics, such as pigments. The pigments can be organic pigments or inorganic pigments, such as one or more of pigment red 57 organic pigment, pigment blue 15 organic pigment and carbon black, preferably pigment red 57 organic pigment, pigment blue 15 organic pigment or carbon black.

[0067] In a preferred embodiment of the present application, the use of the dispersion liquid as described above is specifically provided,

[0068] which comprises the following steps:

[0069] Step (1): adding the pigment powder to be dispersed into the dispersion liquid, stirring uniformly, and then using a homogenizer to strongly beat the slurry to obtain a uniform slurry;

[0070] Step (2): filtering the obtained slurry through a filter screen to obtain a color paste;

[0071] Step (3): testing the stability of the color paste obtained in step (2). Specifically, filtering the color paste obtained in step (2), immediately extracting a sample, testing the particle size and particle size distribution at room temperature, and then sealing the sample in a 60℃ oven for heat preservation, testing the particle size and particle size distribution every three days, and evaluating the stability of the color paste.

[0072] In step (1), the weight ratio of the polymer dispersant to the pigment in the dispersion liquid is (10-120):100, preferably (50-100):100, for example 92:100, 80:100, 72:100 or 60:100.

[0073] In step (1), the beating speed is 5000-15000 rpm, preferably 10000-13000 rpm.

[0074] In step (1), the beating temperature is 20-50°C, preferably 25°C.

[0075] In step (1), the beating time is 1-10 hours, preferably 2-3 hours.

[0076] In step (2), the filter screen size is 200-400 mesh, preferably 300 mesh.

[0077] On the basis of common knowledge in the art, the above-mentioned preferred conditions can be combined arbitrarily, thus obtaining various preferred examples of the present application.

[0078] The reagents and raw materials used in the present application are commercially available.

[0079] The positive progress effect of the present application is that:

[0080] (1) The dispersion liquid of the present application has simple composition, strong and diverse functions, and the amount of polymer dispersant therein is greatly reduced (under the same dispersion condition, the amount of polymer dispersant can be reduced by up to 12%), which can significantly improve the dispersibility and stability of organic pigments in water, and is very suitable for the selection of the cosmetic industry.

[0081] (2) The preparation method of the dispersion liquid of the present application is simple and clear, and has strong operability. DETAILED DESCRIPTION

[0082] The present application will be further described by way of examples, but the present application is not limited in the scope of the examples. In the following examples, the experimental methods not specified in the specific conditions are selected according to the conventional methods and conditions, or according to the instructions of the goods.

[0083] The raw materials used in the following examples and comparative examples are commercially available.

[0084] Example 1

[0085] Preparation of graphene oxide powder

[0086] In a clean 2000 mL beaker, 10 g of graphite oxide and 1000 mL of deionized water were added, stirred for 2 h, then ultrasonic treated for 20 min under 50% ultrasonic power, and stirred for another 30 min, and centrifuged in a high speed centrifuge at 12000 rpm for 40 min. The precipitate was taken out and added into a 1000 mL beaker, and the above stirring, ultrasonic treatment and centrifugation were repeated until the pH of the obtained dispersion was neutral (pH value was 6-7). All the supernatant in the centrifugation was collected, most of the solvent was removed by distillation under reduced pressure, and dried in a vacuum oven at 60°C for 10 h to obtain 8 g of graphene oxide powder, with a yield of about 80%.

[0087] Example 2

[0088] Preparation of a polymer dispersion containing 0.1% graphene oxide and its application

[0089] 57.3 parts of water, 0.3 parts of sodium lauryl sulfate surfactant, 8.0 parts of butanediol as a humectant, and 1 part of phenoxyethanol as a preservative were weighed into a 250 mL beaker, stirred uniformly with a glass rod, then 33.3 parts of a styrene-methyl methacrylate-acrylic acid polymer dispersant (25 g, obtained by copolymerization of styrene, methyl methacrylate, and acrylic acid in a molar ratio of 1:1:1, the method and conditions for preparing the polymer can be conventional in the art, and the molecular weight is 3000-5000) was added, stirred uniformly, then 0.1 part of the graphene oxide powder prepared in Example 1 was added, and a homogenizer was used to stir at a speed of 13000 rpm at room temperature (25°C) for 20 minutes to obtain a dispersion containing 0.1% graphene oxide.

[0090] 25 g of carbon black was weighed into the above dispersion containing 0.1% graphene oxide (total 75.075 g, of which 25 g was styrene-methyl methacrylate-acrylic acid polymer dispersant), stirred uniformly with a glass rod, and a homogenizer was used to stir at a speed of 13000 rpm at room temperature for 2 hours, and then filtered through a 300 mesh sieve to obtain a carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:100 (i.e. the mass of carbon black and polymer dispersant in the paste is the same).

[0091] The amount of polymer dispersant in the dispersion was gradually reduced to 23, 20, 18, and 15 g (i.e. the total weight of the dispersion was kept at 100 parts when preparing the dispersion containing 0.1% graphene oxide, and the reduced amount of polymer dispersant was made up with deionized water), and a carbon black paste was prepared according to the above steps (wherein the mass of carbon black was 25 g), and carbon black pastes with weight ratios of carbon black to polymer dispersant of 100:92, 100:80, 100:72, and 100:60 were successfully prepared.

[0092] Similarly, carbon black was replaced by pigment red 57 organic pigment to prepare pigment red 57 color paste with the weight ratio of pigment red 57 to polymer dispersant being 100:100, 100:92, 100:80, 100:72 and 100:60.

[0093] Similarly, in the dispersion of pigment blue 15 organic pigment, pigment blue 15 color paste with the weight ratio of pigment blue 15 to polymer dispersant being 100:100, 100:92, 100:80, 100:72 and 100:60 was prepared.

[0094] Example 3

[0095] Preparation and application of dispersion liquid containing 0.05% graphene oxide

[0096] Among them, except that the amount of graphene oxide powder prepared in Example 1 is changed to 0.05 parts, and the water is changed to 57.35 parts, the other components remain unchanged, and the dispersion liquid containing 0.05% graphene oxide is prepared according to the method of Example 2. The carbon black color paste with the weight ratio of carbon black to polymer dispersant being 100:100 is prepared according to the same method of Example 2.

[0097] Example 4

[0098] Preparation and application of dispersion liquid containing 0.25% graphene oxide

[0099] Among them, except that the amount of graphene oxide powder prepared in Example 1 is changed to 0.25 parts, and the water is changed to 57.15 parts, the other components remain unchanged, and the dispersion liquid containing 0.25% graphene oxide is prepared according to the method of Example 2. The carbon black color paste with the weight ratio of carbon black to polymer dispersant being 100:100 is prepared according to the same method of Example 2.

[0100] Example 5

[0101] Preparation and application of dispersion liquid containing 0.1% graphene oxide

[0102] The dispersion liquid containing 0.1% graphene oxide was prepared in the same way as in Example 2, except that the type of the polymer dispersant was changed to an acrylic resin polymer (type: J678, manufacturer: BASF, molecular weight: 2000-3000). Carbon black color paste with a weight ratio of carbon black to polymer dispersant of 100:100, 100:92, 100:80, 100:72, and 100:60 was prepared in the same way as in Example 2. Also, pigment red 57 color paste with a weight ratio of pigment red 57 to polymer dispersant of 100:100, 100:92, 100:80, 100:72, and 100:60 was prepared in the same way as in Example 2. Also, pigment blue 15 color paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:100, 100:92, 100:80, 100:72, and 100:60 was prepared in the same way as in Example 2.

[0103] Example 6

[0104] Preparation of dispersion liquid containing 0.1% graphene oxide and its application

[0105] The dispersion liquid containing 0.1% graphene oxide was prepared in the same way as in Example 2, except that the type of the polymer dispersant was changed to an acrylic resin polymer (type: J678, manufacturer: BASF, molecular weight: 2000-3000). Carbon black color paste with a weight ratio of carbon black to polymer dispersant of 100:100, 100:92, 100:80, 100:72, and 100:60 was prepared in the same way as in Example 2. Also, pigment red 57 color paste with a weight ratio of pigment red 57 to polymer dispersant of 100:100, 100:92, 100:80, 100:72, and 100:60 was prepared in the same way as in Example 2. Also, pigment blue 15 color paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:100, 100:92, 100:80, 100:72, and 100:60 was prepared in the same way as in Example 2.

[0106] Comparative Example 1

[0107] Preparation of conventional dispersion liquid not containing graphene oxide and its application

[0108] Take 57.4 parts of water, 0.3 parts of lauryl alcohol sodium sulfate surfactant, 8.0 parts of butanediol and 1 part of phenoxyethanol preservative, place in a 250 mL beaker, stir with a glass rod until uniform, then add 33.3 parts of styrene-methyl methacrylate-acrylic acid polymer dispersant (25 g, obtained by copolymerization of styrene, methyl methacrylate, acrylic acid in a molar ratio of 1:1:1, the method and conditions for preparing the polymer are the same as in Example 2, the molecular weight is 3000-5000), stir until uniform to obtain a conventional dispersion liquid without graphene oxide.

[0109] Take 25 g of carbon black and add it to the above conventional dispersion liquid (total 75.075 g, of which 25 g is styrene-methyl methacrylate-acrylic acid polymer dispersant), stir with a glass rod until uniform, use a homogenizer to stir at 13000 rpm at room temperature for 2 hours, then filter through a 300 mesh screen to obtain a carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:100.

[0110] Gradually reduce the amount of polymer dispersant to 23 g and 20 g, and follow the above steps to prepare the carbon black paste, to obtain a carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:92 and 100:80. However, when the amount of polymer dispersant is further reduced to 18 g, agglomeration occurs and the paste cannot be dispersed, so a carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:72 cannot be prepared. Further reducing the amount of polymer dispersant to 15 g also cannot disperse the paste, so a carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:60 cannot be prepared.

[0111] Similarly, replace the carbon black with pigment red 57 organic pigment to prepare a pigment red 57 paste with a weight ratio of pigment red 57 to polymer dispersant of 100:100, 100:92 and 100:80. However, a pigment red 57 paste with a weight ratio of pigment red 57 to polymer dispersant of 100:72 and 100:60 cannot be prepared.

[0112] Similarly, when dispersing pigment blue 15 organic pigment, a pigment blue 15 paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:100, 100:92 and 100:80 is prepared. However, a pigment blue 15 paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:72 and 100:60 cannot be prepared.

[0113] Comparative Example 2

[0114] Preparation and application of conventional dispersion liquid without graphene oxide

[0115] wherein, except that the kind of the polymer dispersant is changed to methyl acrylate-methacrylic acid polymer (molecular weight is 3000-4000, obtained by copolymerization of methyl acrylate and methacrylic acid at a molar ratio of 1:1, the method and conditions for producing the polymer are the same as in Example 5), the method for preparing the dispersion liquid without graphene oxide is the same as in Comparative Example 1. Carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:100, 100:92, and 100:80 can be prepared in the same manner as in Comparative Example 1, but carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:72 and 100:60 cannot be prepared. Similarly, pigment red 57 paste with a weight ratio of pigment red 57 to polymer dispersant of 100:100, 100:92, and 100:80 can be prepared in the same manner as in Comparative Example 1, but pigment red 57 paste with a weight ratio of pigment red 57 to polymer dispersant of 100:72 and 100:60 cannot be prepared. Pigment blue 15 paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:100, 100:92, and 100:80 can be prepared in the same manner as in Comparative Example 1, but pigment blue 15 paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:72 and 100:60 cannot be prepared.

[0116] Comparative Example 3

[0117] Conventional dispersion liquid preparation without graphene oxide and its application

[0118] wherein, except that the kind of the polymer dispersant is changed to acrylic resin polymer (type J678, manufacturer: BASF, molecular weight is 2000-3000), the method for preparing the dispersion liquid without graphene oxide is the same as in Comparative Example 1. Carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:100, 100:92, and 100:80 can be prepared in the same manner as in Comparative Example 1, but carbon black paste with a weight ratio of carbon black to polymer dispersant of 100:72 and 100:60 cannot be prepared. Similarly, pigment red 57 paste with a weight ratio of pigment red 57 to polymer dispersant of 100:100, 100:92, and 100:80 can be prepared in the same manner as in Comparative Example 1, but pigment red 57 paste with a weight ratio of pigment red 57 to polymer dispersant of 100:72 and 100:60 cannot be prepared. Pigment blue 15 paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:100, 100:92, and 100:80 can be prepared in the same manner as in Comparative Example 1, but pigment blue 15 paste with a weight ratio of pigment blue 15 to polymer dispersant of 100:72 and 100:60 cannot be prepared.

[0119] Effect Example 1

[0120] Tested samples: carbon black dispersions prepared in Example 2, pigment red 57 dispersions, pigment blue 15 dispersions;

[0121] Carbon black dispersions prepared in Example 3;

[0122] Carbon black dispersions prepared in Example 4;

[0123] Carbon black dispersions, pigment red 57 dispersions, pigment blue 15 dispersions prepared in Example 5;

[0124] Carbon black dispersions, pigment red 57 dispersions, pigment blue 15 dispersions prepared in Example 6;

[0125] Carbon black dispersions, pigment red 57 dispersions, pigment blue 15 dispersions prepared in Comparative Example 1;

[0126] Carbon black dispersions, pigment red 57 dispersions, pigment blue 15 dispersions prepared in Comparative Example 2;

[0127] Carbon black dispersions, pigment red 57 dispersions, pigment blue 15 dispersions prepared in Comparative Example 3.

[0128] Test method and conditions: The particle size and particle size distribution of the samples were tested at room temperature by using a laser particle size analyzer (Zetasizer Nano ZS90) with dynamic light scattering method. Then the samples were sealed and placed in an oven at 60°C for incubation. The particle size and particle size distribution were tested every three days to evaluate the stability of the dispersions.

[0129] Test results:

[0130] When the pigment was carbon black, the average particle size of carbon black in the dispersions prepared by dispersing carbon black with the dispersion liquid prepared in Example 2 containing 0.1% oxidized graphene at different ratios of pigment to polymer dispersant was shown in Table 1.

[0131] Table 1

[0132]

[0133] When the pigment was carbon black, the average particle size of carbon black in the dispersions prepared by dispersing carbon black with the dispersion liquid prepared in Comparative Example 1 not containing oxidized graphene at different ratios of pigment to polymer dispersant was shown in Table 2.

[0134] Table 2

[0135]

[0136]

[0137] Note: x in Table 2 represents data not measured

[0138] The average particle size of pigment red 57 in the slurry obtained by dispersing pigment red 57 using the dispersion liquid containing 0.1% graphene oxide prepared in Example 2 at different ratios of pigment to polymeric dispersant is shown in Table 3 below.

[0139] Table 3

[0140]

[0141] The average particle size of pigment red 57 in the slurry obtained by dispersing pigment red 57 using the dispersion liquid containing 0.1% graphene oxide prepared in Example 2 at different ratios of pigment to polymeric dispersant is shown in Table 3 below.

[0142] Table 4

[0143]

[0144] Note: x in Table 4 represents data not measured

[0145] The average particle size of pigment red 57 in the slurry obtained by dispersing pigment red 57 using the dispersion liquid containing 0.1% graphene oxide prepared in Example 2 at different ratios of pigment to polymeric dispersant is shown in Table 3 below.

[0146] Table 5

[0147]

[0148] The average particle size of pigment red 57 in the slurry obtained by dispersing pigment red 57 using the dispersion liquid containing 0.1% graphene oxide prepared in Example 2 at different ratios of pigment to polymeric dispersant is shown in Table 3 below.

[0149] Table 6

[0150]

[0151] Note: x in Table 6 represents data not measured

[0152] The average particle size of pigment red 57 in the slurry obtained by dispersing pigment red 57 using the dispersion liquid containing 0.1% graphene oxide prepared in Example 2 at different ratios of pigment to polymeric dispersant is shown in Table 3 below.

[0153] Table 7

[0154]

[0155] The average particle size of carbon black in the slurry obtained by dispersing carbon black using the dispersion liquid containing no graphene oxide prepared in Comparative Example 2 is shown in Table 8.

[0156] Table 8

[0157]

[0158] Note: x in Table 8 represents data not measured

[0159] The average particle size of pigment red 57 in the slurry obtained by dispersing pigment red 57 using the dispersion liquid containing 0.1% graphene oxide prepared in Example 5 is shown in Table 9.

[0160] Table 9

[0161]

[0162] The average particle size of pigment red 57 in the slurry obtained by dispersing pigment red 57 using the dispersion liquid containing no graphene oxide prepared in Comparative Example 2 is shown in Table 10.

[0163] Table 10

[0164]

[0165] Note: x in Table 10 represents data not measured

[0166] The average particle size of pigment blue 15 in the slurry obtained by dispersing pigment blue 15 using the dispersion liquid containing 0.1% graphene oxide prepared in Example 5 is shown in Table 11.

[0167] Table 11

[0168]

[0169]

[0170] The average particle size of pigment blue 15 in the slurry obtained by dispersing pigment blue 15 using the dispersion liquid containing no graphene oxide prepared in Comparative Example 2 is shown in Table 12.

[0171] Table 12

[0172]

[0173] Note: x in Table 12 represents data not measured

[0174] The average particle size of carbon black in the slurry obtained by dispersing carbon black using the dispersion liquid containing 0.1% graphene oxide prepared in Example 6 is shown in Table 13.

[0175] Table 13

[0176]

[0177]

[0178] The average particle size of carbon black in the slurry obtained by dispersing carbon black using the dispersion liquid containing 0.1% graphene oxide prepared in Example 6 is shown in Table 13.

[0179] Table 13

[0180]

[0181] Note: x in Table 14 represents data not measured

[0182] The average particle size of carbon black in the slurry obtained by dispersing carbon black using the dispersion liquid containing 0.1% graphene oxide prepared in Example 6 is shown in Table 13.

[0183] Table 15

[0184]

[0185] The average particle size of carbon black in the slurry obtained by dispersing carbon black using the dispersion liquid containing 0.1% graphene oxide prepared in Example 6 is shown in Table 13.

[0186] Table 16

[0187]

[0188] Note: x in Table 16 represents data not measured

[0189] The average particle size of carbon black in the slurry obtained by dispersing carbon black using the dispersion liquid containing 0.1% graphene oxide prepared in Example 6 is shown in Table 13.

[0190] Table 17

[0191]

[0192] The average particle size of pigment blue 15 in the slurry obtained by dispersing pigment blue 15 using the dispersion liquid without graphene oxide prepared in Comparative Example 3 at different ratios of pigment to polymer dispersant is shown in Table 18.

[0193] Table 18

[0194]

[0195] Note: x in Table 18 represents data not measured

[0196] It is known in the art that the particle size of pigment in the slurry after dispersion for 10 days is considered to be very good dispersion effect and good stability when the particle size is 110-150 nm, the dispersion effect is good and the stability is good when the particle size is 150-170 nm, and the dispersion effect is not good and the stability is not good when the particle size is greater than 170 nm.

[0197] Based on the above criteria, by comparing and analyzing the data in Tables 1-18, it can be seen that the dispersion effect of the dispersion liquid prepared by adding graphene in Example 2, 5 and 6 is more stable than that of the comparative example under the condition that the amount of polymer dispersant is sufficient.

[0198] Specifically, by comparing and analyzing Tables 1, 7, 13, Tables 3, 9, 15, and Tables 5, 11, 17, it can be seen that the dispersion effect of the dispersion liquid prepared in Example 2 is better than that of the dispersion liquid prepared in Example 5 and 6. That is, when the content of graphene oxide in the dispersion liquid is the same, the type of polymer dispersant in the dispersion liquid can affect the dispersion effect of the dispersion liquid to some extent.

[0199] In addition, by comparing and analyzing Tables 1-6, Tables 7-12, and Tables 13-18, it can be seen that when 100 parts by weight of carbon black, pigment red 57 or pigment blue 15 is dispersed using the dispersion liquid containing 0.1% graphene oxide prepared in Example 2, 5 and 6, only 60 parts by weight of polymer dispersant is needed to obtain a stably dispersed color paste, while when different types of pigments are dispersed using the dispersion liquid without graphene oxide prepared in Comparative Examples 1, 2 and 3, the amount of polymer dispersant is reduced to 72 parts by weight, and the slurry cannot be prepared and the color paste cannot be stably dispersed. It can be seen that the amount of polymer dispersant in the dispersion liquid prepared by the present application is small, the preparation cost is low, and the dispersion effect is good.

[0200] When the pigment is carbon black, the average particle size of carbon black in the slurry obtained by dispersing carbon black using the dispersion liquid prepared in Examples 2-6 and Comparative Examples 1-3 under the condition that the weight ratio of pigment to polymer dispersant is 100:100 is shown in Table 19.

[0201] Table 19

[0202]

[0203] From the data in Table 19, it can be concluded that the addition of hydrophilic graphene has little effect on the particle size of the dispersed pigment when the amount of polymer dispersant is large and sufficient.

[0204] However, in combination with the above evaluation criteria for dispersion effect, further comparative analysis of the particle size data corresponding to Examples 2, 5, and 6 in the table also shows that the dispersion effect of the dispersion liquid prepared in Example 2 is better than that of the dispersion liquids prepared in Examples 5 and 6. That is, when the content of graphene oxide in the dispersion liquid is consistent, the type of polymer dispersant in the dispersion liquid can affect the dispersion effect of the dispersion liquid to some extent.

[0205] In addition, further comparative analysis of the particle size data corresponding to Examples 2, 3, and 4 in the table shows that when the type of polymer dispersant is consistent, the dispersion effect of the dispersion liquid first increases and then decreases with the increase of the content of hydrophilic graphene in the dispersion liquid.

Claims

1. A dispersion, characterized by, Each 100 parts by weight thereof comprises the following components: Polymeric dispersant: 25-35 parts; Hydrophilic graphene: 0.05-1 part; Small molecule surfactant: 0.05-10 parts; and water; The polymeric dispersant is a styrene-methyl methacrylate-acrylic acid polymer; The molecular weight of the polymeric dispersant is 1000-10000; The hydrophilic graphene is graphene oxide.

2. The dispersion of claim 1, wherein The amount of the hydrophilic graphene is 0.05-0.25 parts per 100 parts by weight of the dispersion.

3. The dispersion of claim 2, wherein The amount of the hydrophilic graphene is 0.1 part per 100 parts by weight of the dispersion.

4. The dispersion of claim 1, wherein The molecular weight of the polymeric dispersant is 2000-5000; and / or, the amount of the polymeric dispersant is 33.3 parts per 100 parts by weight of the dispersion.

5. The dispersion of claim 4, wherein The molecular weight of the polymeric dispersant is 2000-3000.

6. The dispersion of claim 4, wherein The molecular weight of the polymeric dispersant is 3000-4000.

7. The dispersion of claim 4, wherein The molecular weight of the polymeric dispersant is 3000-5000.

8. The dispersion of claim 1 wherein, The molecular weight of the small molecule surfactant is below 1000; and / or, the small molecule surfactant is a small molecule anionic surfactant and / or a small molecule nonionic surfactant; and / or, the amount of the small molecule surfactant is 0.05-0.5 parts of the small molecule surfactant per 100 parts by weight of the dispersion; and / or, the amount of water is 50-60 parts per 100 parts by weight of the dispersion.

9. The dispersion of claim 8, wherein The amount of the small molecule surfactant is 0.3 parts of the small molecule surfactant per 100 parts by weight of the dispersion; and / or, the amount of water is 55-58 parts per 100 parts by weight of the dispersion.

10. The dispersion of claim 9, wherein The amount of water is 57.15 parts, 57.3 parts or 57.35 parts per 100 parts by weight of the dispersion.

11. The dispersion of claim 8, wherein The small molecule anionic surfactant is one or more of sodium alkyl benzene sulfonate, sodium lauryl sulfate and lauroyl glutamic acid; and / or, the small molecule nonionic surfactant is a fatty acid glyceride.

12. The dispersion of claim 11, wherein, The small molecule anionic surfactant is sodium lauryl sulfate; and / or, the small molecule nonionic surfactant is a glyceride of stearic acid.

13. The dispersion of any of claims 1-12, wherein, The dispersion further comprises an auxiliary.

14. The dispersion of claim 13, wherein The auxiliary is one or more of a preservative, a humectant and a wetting agent; and / or, the amount of the auxiliary is 0-20 parts per 100 parts by weight of the dispersion.

15. The dispersion of claim 14, wherein The auxiliary is a preservative and a humectant; and / or, the amount of the auxiliary is 0-15 parts per 100 parts by weight of the dispersion.

16. The dispersion of claim 15, wherein The amount of the auxiliary is 0.1-8 parts per 100 parts by weight of the dispersion.

17. The dispersion of claim 14, wherein When the auxiliary comprises a preservative, the preservative is one or more of aromatic alcohols, aromatic acids, fatty alcohols and aldehyde substances; the amount of the preservative is 0-5 parts per 100 parts by weight of the dispersion, but not 0; and / or, when the auxiliary comprises a humectant, the humectant is one or more of polyhydric alcohols, sugars and natural plant extract substances; the amount of the humectant is 0-15 parts per 100 parts by weight of the dispersion, but not 0; And / or, when the auxiliary agent includes a wetting agent, the wetting agent is one or more of sulfonated oil, soy lecithin, mercaptans, hydrazides and organosilicon substances.

18. The dispersion of claim 17, wherein When the auxiliary agent includes a preservative, the preservative is one or more of benzyl alcohol, phenoxyethanol, benzoic acid, salicylic acid and sorbic acid; the amount of the preservative is 0.1-2 parts per 100 parts by weight of the dispersion liquid; And / or, when the humectant includes a sugar, the sugar is one or more of trehalose, sodium hyaluronate and methyl glucose polyether; when the auxiliary agent includes a humectant, the amount of the humectant is 4-10 parts per 100 parts by weight of the dispersion liquid; And / or, when the auxiliary agent includes a wetting agent, the wetting agent is an organosilicon substance.

19. The dispersion of claim 18, wherein When the auxiliary agent includes a preservative, the amount of the preservative is 1 part per 100 parts by weight of the dispersion liquid; And / or, when the auxiliary agent includes a humectant, the humectant is one or more of glycerol, butanediol, polyethylene glycol, propylene glycol, hexylene glycol, xylitol and sorbitol; the amount of the humectant is 6 or 8 parts per 100 parts by weight of the dispersion liquid.

20. The dispersion of claim 19, wherein When the auxiliary agent includes a humectant, the humectant is propylene glycol or butanediol.

21. The dispersion of claim 13, wherein The dispersion liquid includes, per 100 parts by weight: 25-35 parts of a polymeric dispersant, 0.05-0.25 parts of graphene oxide, 0.05-0.5 parts of a small-molecule anionic surfactant and water.

22. The dispersion of claim 13, wherein The dispersion liquid includes, per 100 parts by weight: 25-35 parts of a polymeric dispersant, 0.05-0.25 parts of graphene oxide, 0.05-0.5 parts of a small-molecule anionic surfactant, 0.1-2 parts of a preservative, 4-10 parts of a humectant and 50-60 parts of water.

23. The dispersion of claim 13, wherein The dispersion liquid includes, per 100 parts by weight: 33.3 parts of a styrene-methyl methacrylate-acrylic acid copolymer with a molecular weight of 3000-5000, 0.1 part of graphene oxide, 0.3 part of sodium lauryl sulfate, 1 part of phenoxyethanol and 8 parts of butanediol, and the balance is water.

24. A method of producing the dispersion according to any one of claims 1 to 23, characterized by, It includes the following preparation steps: uniformly mixing the components in the dispersion liquid.

25. The method of producing a dispersion according to claim 24, wherein The preparation method of the hydrophilic graphene includes the following steps: The solution containing the hydrophilic graphite raw material is subjected to several times of "peeling, centrifugation and separation" to obtain supernatant, and the supernatant is dried after removing the solvent in the supernatant; And / or, the mixing device is a homogenizer.

26. The method of producing a dispersion according to claim 25, wherein The peeling method is one or more of stirring, ultrasonic and shearing; And / or, the pH value of the supernatant is 6-7; And / or, the stirring speed of the homogenizer is 1000-15000 rpm; And / or, the stirring time of the homogenizer is 0.5-5 hours; And / or, the stirring temperature of the homogenizer is 0-50℃.

27. The method of claim 26, wherein the dispersion is prepared by The peeling method is stirring and ultrasonic; And / or, the stirring speed of the homogenizer is 10000-13000 rpm; And / or, the stirring time of the homogenizer is 2-3 hours; And / or, the stirring temperature of the homogenizer is 20-30℃.

28. The method of claim 27, wherein the dispersion is prepared by The stirring time of the homogenizer is 2.5 hours; And / or, the stirring temperature of the homogenizer is 25℃.

29. Use of the dispersion of any one of claims 1-23 in the cosmetic industry.

30. Use of the dispersion according to claim 29 in the cosmetic industry, characterized in that, The dispersion is used for dispersing pigments; The pigments are organic pigments or inorganic pigments; And / or, the weight ratio of the polymer dispersant to the pigments in the dispersion is (10-120):

100.

31. Use of the dispersion of claim 30 in the cosmetic industry, wherein the pigments are one or more of Pigment Red 57 organic pigment, Pigment Blue 15 organic pigment, and carbon black; And / or, the weight ratio of the polymer dispersant to the pigments in the dispersion is (50-100):

100.

32. Use of the dispersion of claim 31 in the cosmetic industry, wherein the pigments are Pigment Red 57 organic pigment, Pigment Blue 15 organic pigment, or carbon black; And / or, the weight ratio of the polymer dispersant to the pigments in the dispersion is 92:100, 80:100, 72:100, or 60:100.

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