Method for producing powdery thickener composition

Abstract

To provide a method for producing a powdery thickener composition in improved yield while keeping its thickening effect.SOLUTION: A method for producing a powdery thickener composition includes mixing (A) two or more compounds represented by the formula (1), (B) a glycol-based solvent, and (C) inorganic powder. The (A) two or more compounds have different X's in the formula (1). In at least one of the two or more compounds, R1a or R1b of X in the formula (1) is a compound of alkenyl group. A mixture containing the components (A) and (B) is mixed with the component (C). The formula (1) is: N-X(R2)(R3) [where X is a group represented by R1a or R1b-[CONH-CH2CH2CH2]n-. R1a and R1b each represent an alkyl group or alkenyl group having a predetermined number of carbon atoms. n is an integer of 1-3. R2 and R3 each represent a C1-4 alkyl group or a group represented by -(C2H4O)pH. p is a total of R2 and R3 to represent 0-5].SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present invention relates to a method for producing a powdered thickener composition. [Background technology]

[0002] Thickeners are widely used in foods, cosmetics, and other industrial products, and increase the viscosity of the system by retaining and binding solvents, dispersants, and dispersoids, thereby achieving the appropriate texture required for each application and improving the stability of the system.

[0003] Based on the idea that thickeners hold and restrain solvents, dispersion media, and dispersoids, their molecular design is considered to have structural units that exhibit an interactive force with solvents, dispersion media, and dispersoids. Typical thickeners include cellulose ether-based thickeners, acrylic-based thickeners, polyvinyl alcohol-based thickeners, polyoxyethylene-based thickeners, clay-based thickeners, and surfactant-based thickeners.

[0004] Furthermore, because thickeners exhibit their thickening properties by dissolving or dispersing in a solvent or dispersant, most of them are distributed in powder form, with the solvent or dispersant removed as much as possible, from the standpoint of handling and transportation.

[0005] In hydraulic slurries containing hydraulic powder such as cement, thickeners (rheology modifiers) are sometimes used to improve physical properties such as viscosity and resistance to material separation. Patent Document 1 discloses a rheology modifier characterized by the combined use of two different types of amine oxide surfactants. Patent Document 2 discloses a method of spray-drying an amine oxide together with a carrier salt. Patent Document 3 discloses a method of powdering an aqueous solution or an alcoholic aqueous solution of an amine oxide by supporting it on zeolite. [Prior art documents] [Patent documents]

[0006] [Patent Document 1] Japanese Patent Publication No. 2020-76022 [Patent Document 2] Special Publication No. 49-1443 [Patent Document 3] Japanese Patent Application Publication No. 57-54159 Summary of the Invention [Problem to be solved by the invention]

[0007] Surfactant thickeners form higher-order structures to modify the rheology of aqueous solutions or slurries. Surfactant thickeners, such as amine oxide thickeners, are obtained by oxidation reactions in aqueous systems.

[0008] However, when an amine oxide thickener is synthesized in a form containing water, the formation of a surfactant higher-order structure is promoted due to the interaction between the surfactants, and the viscosity of a solution containing the thickener increases rapidly, resulting in a decrease in the processability of a powdery thickener composition containing the thickener. Therefore, there has been a need for a production method that improves the yield and productivity of a powdery thickener composition containing an amine oxide thickener.

[0009] The present invention provides a method for producing a powdery thickener composition that improves the yield of the powdery thickener composition containing an amine oxide thickener while maintaining the thickening effect of the powdery thickener composition. [Means for solving the problem]

[0010] The present invention provides a method for producing a powdery thickener composition, which comprises mixing (A) two or more compounds represented by the following general formula (1) [hereinafter referred to as component (A)], (B) a glycol-based solvent [hereinafter referred to as component (B)], and (C) an inorganic powder [hereinafter referred to as component (C)], The two or more compounds of (A) have different X's in the general formula (1), and at least one of the two or more compounds has R of X's in the general formula (1). 1a or R 1b is a compound having an alkenyl group, The present invention relates to a method for producing a powdery thickener composition, which comprises mixing a mixture containing components (A) and (B) with component (C). [ka] [Wherein X is R 1a or R 1b -[CONH-CH2CH2CH2] n R is a group represented by the formula 1a R is an alkyl group having 14 to 22 carbon atoms or an alkenyl group having 14 to 22 carbon atoms. 1b is an alkyl group having 13 to 21 carbon atoms or an alkenyl group having 13 to 21 carbon atoms. n is an integer of 1 to 3. 2 and R 3 are each independently an alkyl group having 1 to 4 carbon atoms or -(C2H4O) p H. p is the average number of moles added, and R 2 and R 3 The sum of these is a number between 0 and 5. [Effects of the Invention]

[0011] According to the present invention, it is possible to provide a method for producing a powdery thickener composition that improves the yield of a powdery thickener composition that maintains its thickening effect. DETAILED DESCRIPTION OF THE INVENTION

[0012] In recent years, the Sustainable Development Goals (SDGs) have been proposed to realize a sustainable society. The present invention is believed to be a technology that can contribute to the achievement of SDGs 6, 7, 8, 9, 11, 12, 13, and 14, for example, by improving the chemical economy.

[0013] The inventors have found that by premixing (A) two or more compounds selected from the compounds represented by the above general formula (1) with (B) a glycol-based solvent, and then supporting the resulting mixture on (C) an inorganic powder and powderizing it, the yield of the resulting powdery thickener composition is improved and the thickening effect of the resulting powdery thickener composition is maintained.

[0014] The mechanism by which the yield of the powdery thickener composition obtained by the present invention is improved is not entirely clear, but is presumed to be as follows. As described above, the surfactant high-order structure strongly interacts with the surfactant, causing a significant thickening of the system. The glycol-based solvent, having moderate amphiphilicity, acts as an assistant between water and the surfactant, suppressing an excessive increase in the interaction between the surfactant molecules, thereby reducing the viscosity of the aqueous solution containing the amine oxide-based surfactant, and improving processability and ultimately the yield. Furthermore, the mechanism by which the thickening effect of the powdery thickener composition obtained by the present invention is maintained is not entirely clear, but is speculated as follows. It is known that when a surfactant higher-order structure incorporates an oily substance, the interaction between surfactants decreases, resulting in a reduced thickening effect. It is believed that, due to its sufficient hydrophilicity, when added as a powdery thickener composition to a solution or dispersion to be thickened, the glycol-based solvent migrates preferentially into bulk water compared to the surfactant higher-order structure, thereby restoring the interaction between surfactant molecules and exhibiting a high thickening effect. However, the present invention is not limited to this mechanism of action.

[0015] First, the components used in the method for producing the powdery thickener composition of the present invention will be described. In the present invention, a powdery thickener composition (hereinafter referred to as the powdery thickener composition of the present invention) is produced by mixing multiple components including (A) two or more types of compounds represented by the above general formula (1) [hereinafter referred to as component (A)], (B) a glycol-based solvent [hereinafter referred to as component (B)], and (C) an inorganic powder [hereinafter referred to as component (C)].

[0016] The component (A) is two or more compounds selected from the compounds represented by the general formula (1) (hereinafter also referred to as compound (1)). The two or more compounds of the component (A) have different X's in the general formula (1), and at least one of the two or more compounds has a different R of X's in the general formula (1). 1a or R 1b is a compound having an alkenyl group.

[0017] Regarding the compound (1), when X in the general formula (1) is different, for example, when there are two kinds of compound (1), the following embodiments can be mentioned. In the following embodiments, R of at least one of the two kinds of compound (1) is different. 1a or R 1b is an alkenyl group. (i) One R 1a or R 1b is an alkyl group, and the other R 1a or R 1b is an alkenyl group. (ii) One R 1a or R 1b The number of carbon atoms in the other R 1a or R 1b The carbon numbers are different. (iii) One of the Xs is R 1a and the other X is R 1b -[CONH-CH2CH2CH2] n -It is. (iv) Both X and R 1b -[CONH-CH2CH2CH2] n - and one n is different from the other n. (v) A combination of (i) to (iv) above.

[0018] In the general formula (1), X is R 1a or R 1b -[CONH-CH2CH2CH2] n - is a group represented by the formula: R 1a is an alkyl group having 14 to 22 carbon atoms or an alkenyl group having 14 to 22 carbon atoms. R 1a When is an alkenyl group, it preferably has 18 or more carbon atoms and preferably 22 or less carbon atoms. R 1a When is an alkyl group, it preferably has 16 or more carbon atoms and preferably has 22 or less carbon atoms. R 1b is an alkyl group having 13 to 21 carbon atoms or an alkenyl group having 13 to 21 carbon atoms. R 1b When is an alkenyl group, it preferably has 17 or more carbon atoms and preferably 21 or less carbon atoms. R 1b When is an alkyl group, it preferably has 15 or more carbon atoms and preferably 21 or less carbon atoms. n is preferably 0 or 1. R 2 and R 3 are each independently preferably an alkyl group having 1 to 2 carbon atoms or -(C2H4O) p It is a group represented by H. p is preferably a number between 0 and 3.

[0019] The powdery thickener composition of the present invention contains two or more, preferably five or less, more preferably two, compounds (1) having different X's in general formula (1). At least one of the two or more compounds (1) contained in the powdery thickener composition has a different R of X's in general formula (1). 1a or R 1b is an alkenyl group having 14 to 22 carbon atoms, that is, R in X in general formula (1) 1a an alkenyl group having 14 to 22 carbon atoms as R 1b It is a compound containing an alkenyl group having 13 to 21 carbon atoms as the alkyl group.

[0020] In the present invention, there are two types of compound (1), and one of the two types of compound (1), including the above (i) to (v), is a compound in which X in the general formula (1) is R 1a and a compound having an alkenyl group with a carbon number of 14 to 22. That is, the component (A) is two compounds selected from the compounds represented by the general formula (1), and the two compounds of the component (A) have different X in the general formula (1), and one of the two compounds has X in the general formula (1) that is R 1a and R 1a is an alkenyl group.

[0021] The component (A) is a compound in which X in the general formula (1) is R 1a or R 1b-[CONH-CH2CH2CH2] n - (wherein R 1a is an alkenyl group having 14 to 22 carbon atoms, and R 1b is an alkenyl group having from 13 to 21 carbon atoms), and compound (1b) in which X in general formula (1) is different from compound (1a). Specifically, the component (A) may include a compound (1a) represented by the following general formula (1a) and a compound (1b) represented by the following general formula (1b).

[0022] [ka]

[0023] [During the ceremony, n1 and n2 each independently represent an integer of 0 or more and 3 or less. R 11a When n1 is 0, it is an alkenyl group having 14 to 22 carbon atoms, and when n1 is 1 to 3, it is an alkenyl group having 13 to 21 carbon atoms. R 11b When n2 is 0, it is an alkyl group having 14 to 22 carbon atoms or an alkenyl group having 14 to 22 carbon atoms, and when n2 is 1 to 3, it is an alkyl group having 13 to 21 carbon atoms or an alkenyl group having 13 to 21 carbon atoms. However, if n1 and n2 are the same number, R 11b The alkenyl group in R 11a is an alkenyl group different from R 2 and R 3 are each independently an alkyl group having 1 to 4 carbon atoms or -(C2H4O) p H. p is the average number of moles added, and R 2 and R 3 The sum of these is a number between 0 and 5.

[0024] In general formula (1a), R 11a The number of carbon atoms is preferably 17 or more and preferably 22 or less. In the general formula (1a), n1 is preferably 0 or 1, and more preferably 0.

[0025] In the general formula (1b), n2 is 0 and R 11b When is an alkyl group, R 11b The number of carbon atoms is preferably 16 or more and preferably 22 or less. In the general formula (1b), n2 is 0 and R 11b When is an alkenyl group, R 11b The number of carbon atoms is preferably 18 or more and preferably 22 or less. In the general formula (1b), n2 is 1 to 3 and R 11b When is an alkyl group, R 11b The number of carbon atoms is preferably 15 or more and preferably 21 or less. In the general formula (1b), n2 is 1 to 3 and R 11b When is an alkenyl group, R 11b The number of carbon atoms is preferably 17 or more and preferably 21 or less. In general formula (1b), R 11b is preferably an alkyl group. In the general formula (1b), n2 is preferably 0 or 1.

[0026] In general formula (1a) or (1b), R 2 and R 3 are each independently preferably an alkyl group having 1 or 2 carbon atoms or -(C2H4O) p It is a group represented by H, and more preferably an alkyl group having 1 or 2 carbon atoms. In the general formula (1a) or (1b), p is preferably a number of 0 or more and 3 or less. If n1 and n2 are the same number, R 11b The alkenyl group in R 11a is an alkenyl group different from

[0027] A preferred embodiment of the component (A) of the present invention includes a compound (11a) represented by the following general formula (11a) and a compound (1b) represented by the following general formula (1b).

[0028] [ka]

[0029] [During the ceremony, n2 is an integer between 0 and 3 inclusive. R 11a is an alkenyl group having 14 to 22 carbon atoms. R 11b When n2 is 0, it is an alkyl group having 14 to 22 carbon atoms or an alkenyl group having 14 to 22 carbon atoms, and when n2 is 1 to 3, it is an alkyl group having 13 to 21 carbon atoms or an alkenyl group having 13 to 21 carbon atoms. However, if n2 is 0, R 11b The alkenyl group in R 11a is an alkenyl group different from R 2 and R 3 are each independently an alkyl group having 1 to 4 carbon atoms or -(C2H4O) p H. p is the average number of moles added, and R 2 and R 3 The sum of these is a number between 0 and 5.

[0030] The compound (11a) represented by the general formula (11a) corresponds to the compound in which n1 is 0 in the general formula (1a). 11a , R 2 and R 3 The preferred embodiments of the compound (1b) are the same as those of the general formula (1a). In this combination, the preferred embodiments of the compound (1b) are the same as those of the general formula (1a).

[0031] In component (A), the mass ratio of compound (1b) / compound (1a) is preferably 5 / 95 or more, more preferably 25 / 75 or more, even more preferably 40 / 60 or more, and is preferably 95 / 5 or less, more preferably 75 / 25 or less, even more preferably 60 / 40 or less, from the viewpoint of obtaining a rheology-modifying effect, for example, high viscoelasticity, over a wider temperature range.

[0032] In component (A), the mass ratio of compound (1b) / compound (11a) is preferably 5 / 95 or more, more preferably 25 / 75 or more, even more preferably 40 / 60 or more, and is preferably 95 / 5 or less, more preferably 75 / 25 or less, even more preferably 60 / 40 or less, from the viewpoint of obtaining a rheology-modifying effect, for example, high viscoelasticity, over a wider temperature range.

[0033] The powdery thickener composition of the present invention preferably contains a small amount of compounds having a structure similar to that of compound (1) and having an alkyl group or alkenyl group with a small number of carbon atoms. Specifically, it is preferable that the content of amine oxides having an alkyl group with less than 14 carbon atoms, an alkenyl group with less than 14 carbon atoms, or an acyl group with less than 14 carbon atoms (hereinafter also referred to as short-chain amine oxides) is small. The powdery thickener composition of the present invention preferably has a mass ratio of the total content of short-chain amine oxides to the total content of compound (1) of 50 / 50 or less, more preferably 25 / 75 or less, even more preferably 10 / 90 or less, and even more preferably 0 / 100, i.e., does not contain any short-chain amine oxides. For convenience, when considered in terms of general formula (1), a short-chain amine oxide is a compound represented by the formula: 1a is an alkyl group having less than 14 carbon atoms or an alkenyl group having less than 14 carbon atoms, and 1b is an alkyl group having less than 13 carbon atoms or an alkenyl group having less than 13 carbon atoms.

[0034] Component (B) is a glycol-based solvent. Component (B) may be a glycol-based solvent having two hydroxyl groups. Component (B) may be a diol having 2 to 10 carbon atoms. Examples of component (B) include propylene glycol, ethylene glycol, dipropylene glycol, 2-methyl-2,4-pentanediol, and 1,3-butanediol. From the viewpoint of the thickening properties of the powdery thickener composition, component (B) is preferably propylene glycol, ethylene glycol, or dipropylene glycol, and more preferably propylene glycol or ethylene glycol.

[0035] Component (C) is an inorganic powder. Examples of component (C) include powders of inorganic salts such as calcium carbonate and calcium silicate, powders of clay minerals such as kaolinite and bentonite, fine powders of blast furnace slag and fly ash, sodium sulfate, aluminum sulfate, zeolite, calcium hydroxide, magnesium hydroxide, aluminum hydroxide, silica powder (including fine silica powder and porous silica powder), and any combination thereof. Component (C) is preferably an inorganic powder capable of supporting a liquid. From the viewpoint of anti-caking properties, powders of inorganic salts such as silica powder (including fine silica powder and porous silica powder), calcium carbonate, and calcium silicate are preferred, and silica powder (including fine silica powder and porous silica powder) is more preferred.

[0036] In the present invention, the term "having the ability to support liquid" for component (C) means that the oil absorption capacity according to the method described in JIS K6220(-1995) is 100 ml / 100 g or more. The oil absorption capacity of component (B) is preferably 200 ml / 100 g or more, and preferably 450 ml / 100 g or less, more preferably 350 ml / 100 g or less.

[0037] The average particle size of component (C) is preferably at least 5 μm, more preferably at least 10 μm, and is preferably no greater than 200 μm, more preferably no greater than 100 μm. This average particle size is calculated on a volume basis and is a value measured using a laser diffraction flow distribution analyzer LA-920 (manufactured by Horiba, Ltd.).

[0038] From the viewpoint of miscibility, the specific surface area of ​​component (C) is preferably 50 m 2 / g or more, more preferably 100m 2 / g or more, and from the viewpoint of oil absorption capacity, preferably 300m 2 / g or less, more preferably 200m 2 / g or less. This specific surface area was measured using a fully automatic specific surface area measuring device, Macsorb HM-model 1201 (manufactured by Mountec Co., Ltd.).

[0039] The amorphous silica of component (C) can be, for example, synthetic amorphous silica commercially available as Nipsil NS-K (manufactured by Tosoh Silica Corporation). Here, amorphous silica refers to silica that has a network structure of Si-O and does not have a fixed crystalline structure.

[0040] <Composition and optional components of the powdery thickener composition of the present invention> In the powdery thickener composition of the present invention, the content of component (A) is preferably 2% by mass or more, more preferably 4% by mass or more, even more preferably 6% by mass or more, still more preferably 8% by mass or more, and even more preferably 10% by mass or more, from the viewpoint of the yield of the powdery thickener composition, and is preferably 60% by mass or less, more preferably 50% by mass or less, even more preferably 40% by mass or less, still more preferably 30% by mass or less, still more preferably 20% by mass or less, and even more preferably 15% by mass or less, from the viewpoint of the flowability of the powdery thickener composition.

[0041] In the powdery thickener composition of the present invention, the content of component (B) is preferably 1% by mass or more, more preferably 10% by mass or more, and even more preferably 20% by mass or more from the viewpoint of productivity, and is preferably 50% by mass or less, more preferably 40% by mass or less, and even more preferably 30% by mass or less from the viewpoint of thickening properties.

[0042] In the powdery thickener composition of the present invention, the mass ratio (A) / (B) of the content of component (A) to the content of component (B) is preferably 0.10 or more, more preferably 0.20 or more, even more preferably 0.30 or more, and still more preferably 0.40 or more, from the viewpoint of the yield of the powdery thickener composition, and is preferably 5.00 or less, more preferably 2.00 or less, even more preferably 1.00 or less, still more preferably 0.80 or less, still more preferably 0.70 or less, and still more preferably 0.65 or less, from the viewpoint of the yield of the powdery thickener composition.

[0043] In the powdery thickener composition of the present invention, the content of component (C) is preferably 10% by mass or more, more preferably 20% by mass or more, and even more preferably 30% by mass or more, from the viewpoint of the fluidity of the powdery thickener composition, and is preferably 70% by mass or less, more preferably 60% by mass or less, and even more preferably 50% by mass or less, from the viewpoint of thickening properties.

[0044] The powdery thickener composition of the present invention may optionally contain (D) an anionic aromatic compound (hereinafter referred to as component (D)). Component (D) is an anionic aromatic compound. Examples of component (D) include one or more compounds selected from sulfonic acids having an aromatic ring, carboxylic acids having an aromatic ring, phosphonic acids having an aromatic ring, and salts thereof. Examples of salts of component (D) include alkali metal salts such as sodium salts and potassium salts, and alkaline earth metal salts such as calcium salts. Component (D) is preferably an acid-type compound having a total carbon number of 6 to 12. Specific examples of component (D) include salicylic acid, p-toluenesulfonic acid, sulfosalicylic acid, benzoic acid, m-sulfobenzoic acid, p-sulfobenzoic acid, 4-sulfophthalic acid, 5-sulfoisophthalic acid, p-phenolsulfonic acid, m-xylene-4-sulfonic acid, cumenesulfonic acid, methylsalicylic acid, styrenesulfonic acid, and chlorobenzoic acid. These may form salts. Two or more types of component (D) may be used. Component (D) is preferably one or more compounds selected from sulfonic acids having an aromatic ring, carboxylic acids having an aromatic ring, and salts thereof.

[0045] When the powdery thickener composition of the present invention contains component (D), the content of component (D) in the composition is preferably 1.0 mass% or more, more preferably 1.5 mass% or more, and even more preferably 2.0 mass% or more from the viewpoint of thickening properties, and is preferably 10.0 mass% or less, more preferably 7.5 mass% or less, and even more preferably 5.0 mass% or less from the viewpoint of storage stability.

[0046] The powdery thickener composition of the present invention may optionally contain (E) a water-soluble polymer compound (hereinafter referred to as component (E)). Component (E) may include (E1) a nonionic polymer compound such as polyalkylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, or alcohol alkoxylate, or (E2) a cationic polymer compound such as polyamidepolyamine / epichlorohydrin condensate, dimethylamine / ammonia / epichlorohydrin condensate, dimethylamine / trimethylamine / epichlorohydrin condensate, vinylpyrrolidone / quaternized dimethylaminoethyl methacrylate copolymer, quaternized polyethyleneimine to which a polyoxyalkylene group may be added, or vinylpyrrolidone / alkylaminoacrylate copolymer. The polyvinyl alcohol may be a fully saponified polyvinyl alcohol or a partially unsaponified polyvinyl alcohol, for example, an intermediately saponified polyvinyl alcohol or a partially saponified polyvinyl alcohol, with a partially saponified polyvinyl alcohol being preferred. The alcohol alkoxylate may be an ether compound having a hydrocarbon group, preferably a hydrocarbon group having from 10 to 22 carbon atoms, and a polyoxyalkylene group having an average addition molar number of from 9 to 5,000. From the viewpoint of versatility, component (E) is preferably one or more polymeric compounds selected from polyalkylene glycol, polyvinyl alcohol, and polyvinylpyrrolidone, more preferably polyalkylene glycol and polyvinyl alcohol, and even more preferably polyethylene glycol, polypropylene glycol, a copolymer of ethylene oxide and propylene oxide, and polyvinyl alcohol. In the component (E), water soluble means that the polymer compound dissolves in an amount of 1 g or more in 100 g of water at 20°C.

[0047] From the viewpoint of versatility, the weight-average molecular weight of component (E) is preferably 500 or more, more preferably 1,000 or more, and even more preferably 2,000 or more, and from the viewpoint of rheology-modifying effect, it is preferably 200,000 or less, more preferably 150,000 or less, even more preferably 100,000 or less, still more preferably 30,000 or less, and even more preferably 5,000 or less. The weight-average molecular weight of component (E) was measured by gel permeation chromatography (GPC) under the following conditions. *GPC conditions Apparatus: GPC (HLC-8320GPC) manufactured by Tosoh Corporation Column: G4000PWXL + G2500PWXL (Tosoh Corporation) Eluent: 0.2M phosphate buffer / CH3CN=9 / 1 Flow rate: 1.0mL / min Column temperature: 40℃ Detection: RI Sample size: 0.2 mg / mL Standard substance: Polyethylene glycol equivalent (monodisperse polyethylene glycol: molecular weight 250,000, 145,000, 87,500, 46,000, 24,000)

[0048] When the powdery thickener composition of the present invention contains component (E), the content of component (E) in the composition is preferably 1% by mass or more, more preferably 5% by mass or more, and even more preferably 10% by mass or more from the viewpoint of versatility, and is preferably 50% by mass or less, more preferably 40% by mass or less, and even more preferably 30% by mass or less from the viewpoint of thickening properties.

[0049] The powdery thickener composition of the present invention may optionally contain a cement wetting agent, an expanding agent, a waterproofing agent, a retarder, a quick-setting agent, a foaming agent, a foaming agent, a waterproofing agent, a superplasticizer, a thickener other than the powdery thickener composition of the present invention, a flocculating agent, a drying shrinkage-reducing agent, a strength-enhancing agent, a hardening accelerator, a preservative, an antifoaming agent, a dispersant, water, and a solvent other than component (B). The water may be water mixed in during the production of component (A).

[0050] <Method of producing powdery thickener composition> The method for producing a powdery thickener composition of the present invention is a method for producing a powdery thickener composition by mixing (A) two or more compounds represented by the above general formula (1), (B) a glycol-based solvent, and (C) an inorganic powder, The two or more compounds of (A) have different X's in the general formula (1), and at least one of the two or more compounds has R of X's in the general formula (1). 1a or R 1b is a compound having an alkenyl group, The mixture containing component (A) and component (B) is mixed with component (C).

[0051] In the method for producing the powdery thickener composition of the present invention, first, component (A) and component (B) are mixed to obtain a mixture of component (A) and component (B). Component (A) may be used in a composition containing component (A) and water. In other words, component (A) may contain water that is mixed in during the synthesis of component (A).

[0052] The amount of component (A) mixed relative to the total amount of mixed components used in the production of the powdery thickener composition is, from the viewpoint of the yield of the powdery thickener composition, preferably 2% by mass or more, more preferably 4% by mass or more, even more preferably 6% by mass or more, even more preferably 8% by mass or more, and even more preferably 10% by mass or more, and from the viewpoint of the flowability of the powdery thickener composition, preferably 60% by mass or less, more preferably 50% by mass or less, even more preferably 40% by mass or less, even more preferably 30% by mass or less, even more preferably 20% by mass or less, and even more preferably 15% by mass or less.

[0053] The amount of component (B) mixed is preferably 1% by mass or more, more preferably 10% by mass or more, and even more preferably 20% by mass or more, based on the total amount of mixed components used in the production of the powdered thickener composition, from the viewpoint of powdering efficiency, and is preferably 50% by mass or less, more preferably 40% by mass or less, and even more preferably 30% by mass or less, from the viewpoint of thickening properties.

[0054] The mass ratio (A) / (B) of the amount of component (A) mixed to the amount of component (B) mixed is preferably 0.10 or more, more preferably 0.20 or more, even more preferably 0.30 or more, and even more preferably 0.40 or more, from the viewpoint of the yield of the powdery thickener composition, and is preferably 5.00 or less, more preferably 2.00 or less, even more preferably 1.00 or less, even more preferably 0.80 or less, even more preferably 0.70 or less, and even more preferably 0.65 or less, from the viewpoint of the yield of the powdery thickener composition.

[0055] In a mixture containing components (A) and (B) that is to be mixed with component (C), the amount of component (A) mixed is preferably 5% by mass or more, more preferably 10% by mass or more, and even more preferably 15% by mass or more from the viewpoint of thickening, and is preferably 60% by mass or less, more preferably 40% by mass or less, and even more preferably 20% by mass or less from the viewpoint of productivity. In the mixture, the component other than components (A) and (B) may be water.

[0056] In a mixture containing the (A) component and the (B) component, which is to be mixed with the (C) component, the amount of the (B) component mixed is preferably 10% by mass or more, more preferably 20% by mass or more, and even more preferably 30% by mass or more, from the viewpoint of productivity, and is preferably 90% by mass or less, more preferably 70% by mass or less, and even more preferably 50% by mass or less, from the viewpoint of thickening properties.

[0057] In the method for producing a powdery thickener composition of the present invention, a mixture containing components (A) and (B) is then mixed with component (C). In the present invention, by mixing a mixture of components (A) and (B) with component (C), the yield of a powdery thickener composition that maintains its thickening effect is improved. The order in which components (D) and (E) are mixed is not particularly limited, but for example, when component (D) is used, it is preferable to mix a mixture containing components (A), (B), and (D) with component (C). Also, when component (E) is used, it is preferable to mix components (C) and (E) first, and then mix a mixture containing components (A) and (B).

[0058] The amount of component (C) mixed relative to the total amount of mixed components used in producing the powdered thickener composition is preferably 10% by mass or more, more preferably 20% by mass or more, and even more preferably 30% by mass or more, from the viewpoint of the fluidity of the powdered thickener composition, and is preferably 70% by mass or less, more preferably 60% by mass or less, and even more preferably 50% by mass or less, from the viewpoint of thickening properties.

[0059] The amount of component (D) mixed, relative to the total amount of mixed components used in the production of the powdery thickener composition, is preferably 1.0 mass% or more, more preferably 1.5 mass% or more, and even more preferably 2.0 mass% or more, from the viewpoint of thickening properties, and is preferably 10.0 mass% or less, more preferably 7.5 mass% or less, and even more preferably 5.0 mass% or less, from the viewpoint of storage stability.

[0060] The amount of component (E) mixed relative to the total amount of mixed components used in the production of the powdery thickener composition is preferably 1% by mass or more, more preferably 5% by mass or more, and even more preferably 10% by mass or more, from the viewpoint of versatility, and is preferably 50% by mass or less, more preferably 40% by mass or less, and even more preferably 30% by mass or less, from the viewpoint of thickening properties.

[0061] In the method for producing the powdery thickener composition of the present invention, a liquid component containing the (A) component and the (B) component and a powdery component containing the (C) component are prepared, and the liquid component and the powdery component are mixed to produce the powdery thickener composition. The liquid component may optionally contain component (D), and the powder component may optionally contain component (E).

[0062] When a powdery thickener composition is produced by mixing a liquid component containing components (A) and (B) with a powdery component containing component (C), the mass ratio of the mixed amounts of the liquid component to the powdery component, (liquid component) / (powdered component), is preferably 0.1 or more, more preferably 0.3 or more, even more preferably 0.5 or more, from the viewpoint of thickening property, and is preferably 5.0 or less, more preferably 3.0 or less, even more preferably 2.0 or less, and even more preferably 1.0 or less, from the viewpoint of flowability of the powdery thickener composition. The mass of the liquid component may be the sum of the mixed amounts of components (A), (B), (D), and water mixed in during synthesis of component (A), and the mass of the powdery component may be the sum of the mixed amounts of components (C) and (E).

[0063] In the method for producing the powdery thickener composition of the present invention, optionally, cement wetting agents, expanding agents, waterproofing agents, retarders, quick-setting agents, foaming agents, foaming agents, waterproofing agents, fluidizing agents, thickeners other than the powdery thickener composition of the present invention, flocculants, drying shrinkage reducing agents, strength enhancers, hardening accelerators, preservatives, antifoaming agents, and dispersants may be mixed.

[0064] The powdery thickener composition obtained by the method for producing a powdery thickener composition of the present invention has improved water dispersibility. The powdery thickener composition of the present invention is useful as a thickener for, for example, hydraulic slurry compositions, coating compositions, electronic material compositions, polishing compositions, ejection compositions, pharmaceutical compositions, and sanitary compositions. [Example]

[0065] <Example 1 and Comparative Example 1> In Example 1 and Comparative Example 1, the following (A) amphoteric surfactant, (B) glycol-based solvent, (B') comparative solvent, (C) inorganic powder, (D) anionic aromatic compound, (E) water-soluble polymer compound, and other components were used.

[0066] (1) Components used in the preparation of the powdered thickener composition <Liquid ingredients> (A) Amphoteric surfactant (a-1): oleyldimethylamine oxide (in general formula (1a), R 11a : Alkenyl group with 18 carbon atoms (oleyl group), n1: 0, R 2 : Methyl group, R 3 : methyl group) (a-2): Oleic acid amide propyl dimethylamine oxide (in general formula (1a), R 11a : Alkenyl group having 17 carbon atoms, n1:1, R 2 : Methyl group, R 3 : methyl group) The component (A) used was a composition containing 30% by mass of effective solids and water. (B) Glycol-based solvent (b-1): Propylene glycol (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) (b-2): Ethylene glycol (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) (b-3): Dipropylene glycol (mixture of isomers) (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) (b-4): 2-methyl-2,4-pentanediol (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) (b-5): 1,3-butanediol (Fujifilm Wako Pure Chemical Industries, Ltd.) (B'-1) Comparative solvent (b'-1): Methanol (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) (b'-2): 1-propanol (Fujifilm Wako Pure Chemical Industries, Ltd.) (b'-3): Benzyl alcohol (Fujifilm Wako Pure Chemical Industries, Ltd.) (b'-4): 2-phenoxyethanol (Fujifilm Wako Pure Chemical Industries, Ltd.) (b'-5): Diethylene glycol monobutyl ether (Tokyo Chemical Industry Co., Ltd.) (D) Anionic aromatic compounds (d-1): Sodium meta-xylene sulfonate monohydrate crystals, SXS-Y (manufactured by Itochu Chemical Frontier Corporation)

[0067] <Powdered ingredients> (C) Inorganic powder (c-1): Silica powder, Nipsil NS-K (manufactured by Tosoh Silica Corporation) (c-2): Ground blast furnace slag, Esment 4000 (manufactured by Nippon Steel Blast Furnace Cement Co., Ltd.) (E) Water-soluble polymer compound (e-1): Polyethylene glycol 4,000 (Fujifilm Wako Pure Chemical Industries, Ltd.) ·(e-2):Poly(ethylene oxide) average MV 200,000,powder(Merck KGaA)

[0068] (2) Method for producing powdery thickener composition First, a liquid component was prepared containing the components (A), (B), and (D) in the proportions shown in Table 1. Specifically, the components shown in Table 1 were placed in a glass flask and mixed for 10 minutes to prepare a liquid component containing the components (A) and (B). Next, a powdered component prepared by blending component (C) or component (C) and component (E) in the ratio shown in Table 1 with respect to the powdered thickener composition was mixed for 10 seconds using a coffee mill GCM-56 (Device Style Holdings) to prepare a powdered component containing component (C). The liquid component was added to the obtained powder component and mixed for another minute until the powder became homogeneous, to produce a powdered thickener composition, which had been passed through a sieve with 600 μm openings.

[0069] (3) Calculation of the yield of the powdery thickener composition The yield (%) of the powdery thickener composition produced by the method described in (2) was calculated based on the following formula: The results are shown in Table 1. Yield (%) = [mass (g) of powdered thickener composition passing through a sieve with 600 μm openings × 100] / [mass (g) of raw materials used in producing the powdered thickener composition]

[0070] <Preparation of cement slurry> At 20°C, 400 g of water and 400 g of cement (ordinary Portland cement, manufactured by Taiheiyo Cement Corporation) were mixed and stirred for 30 seconds using a commercially available hand mixer. Thereafter, 4 g of each of the powdered thickener compositions described in Example 1 and Comparative Example 1 was added, and stirring was continued for an additional 3 minutes to prepare a hydraulic slurry composition.

[0071] <Measurement of Viscosity of Hydraulic Slurry Composition> The viscosity of the obtained hydraulic slurry composition was measured at 20° C. using a Brookfield viscometer (manufactured by RION Corporation, VISCOTESTER VT-04E, rotor No. 1, rotation speed: 62.5 rpm). The results are shown in Table 1.

[0072] [Table 1]

[0073] *1: In the table, component (a-1), component (a-2), and component (a'-1) each represent the mixed amount of a composition containing 30% by mass of effective solids and water. *2: Comparative Example 1-10 was prepared by mixing components (A) and (B) separately with component (C).

[0074] In Table 1, Examples 1-1 to 1-9 showed higher yields and better slurry viscosities than Comparative Examples 1-1 to 1-10. This is thought to be because the glycol-based solvent prevented excessive increases in the interaction between surfactant molecules.

Claims

1. A method for producing a powdery thickener composition, comprising mixing (A) two or more compounds represented by the following general formula (1) [hereinafter referred to as component (A)], (B) a glycol-based solvent [hereinafter referred to as component (B)], and (C) an inorganic powder [hereinafter referred to as component (C)], The component (A) includes a compound (11a) represented by the following general formula (11a) and a compound (1b) represented by the following general formula (1b): the component (B) is propylene glycol, ethylene glycol, dipropylene glycol, 2-methyl-2,4-pentanediol, or 1,3-butanediol; The component (C) is a silica powder, the mass ratio (A) / (B) of the amount of the component (A) mixed to the amount of the component (B) mixed is 0.30 or more and 0.80 or less; A liquid component containing the components (A) and (B) and a powder component containing the component (C) are mixed together such that the mass ratio of the liquid component to the powder component is 0.5 or more and 2.0 or less, in terms of the mass ratio of the liquid component / powder component. Method for producing a powdered thickener composition. 【Chemistry 1】 [Wherein X is R １ａ or R １ｂ -[CONH-CH ２ CH ２ CH ２ ] ｎ - is a group represented by R １ａ is an alkyl group having 14 to 22 carbon atoms or an alkenyl group having 14 to 22 carbon atoms. １ｂ is an alkyl group having 13 to 21 carbon atoms or an alkenyl group having 13 to 21 carbon atoms. n is an integer of 1 to 3. ２ and R ３ are each independently an alkyl group having 1 to 4 carbon atoms or -(C ２ H ４ O) ｐ H. p is the average number of moles added, and R ２ and R ３ The sum of these is a number between 0 and 5. 【Chemistry 2】 [During the ceremony, n2 is an integer of 1 or more and 3 or less. R 11a is an alkenyl group having 14 to 22 carbon atoms. R 11b is an alkyl group having 13 to 21 carbon atoms or an alkenyl group having 13 to 21 carbon atoms. R 2 and R 3 are each independently an alkyl group having 1 to 4 carbon atoms or a group represented by —(C 2 H 4 O) pH. p is the average number of moles added, and the total of R 2 and R 3 is a number of 0 to 5.

2. The method for producing a powdery thickener composition according to claim 1 , wherein the liquid component further comprises (D) an anionic aromatic compound.

3. The method for producing a powdery thickener composition according to claim 1 or 2, wherein the powdery component further comprises (E) a water-soluble polymer compound.

4. A method for producing a powdered thickener composition described in any one of claims 1 to 3, wherein the mixed amount of component (A) is 2% by mass or more and 60% by mass or less of the total mixed components used in producing the powdered thickener composition.

5. A method for producing a powdered thickener composition described in any one of claims 1 to 4, wherein the amount of component (B) mixed is 1 mass% or more and 50 mass% or less of the total amount of mixed components used in producing the powdered thickener composition.

6. A method for producing a powdered thickener composition described in any one of claims 1 to 5, wherein the mixed amount of component (C) is 10% by mass or more and 70% by mass or less of the total mixed components used in producing the powdered thickener composition.

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