Anti-segregation agent, preparation method and application

Abstract

The invention discloses an anti-segregation agent, a preparation method and application, and relates to the technical field of concrete admixtures. The anti-segregation agent comprises a dispersing agent, a thickening agent and a preservative; the dispersing agent comprises a copolymer obtained from a reaction monomer under the action of an initiator; the reaction monomer comprises an unsaturated carboxylic acid monomer and a first monomer; wherein the first monomer comprises at least one of a sulfonic acid monomer, an organic silicon monomer, an aromatic monomer and a phosphate ester monomer. The anti-segregation agent disclosed by the invention is wider in application range to concrete aggregate, wider in upper and lower limit range of a concrete segregation state, higher in regulation capability to a concrete mixture, more flexible in addition and use modes and lower in production cost.

Description

Technical Field

[0001] The present invention relates to the technical field of concrete admixtures, and in particular to an anti-segregation agent, a preparation method and application thereof. Background Art

[0002] The segregation of concrete is a technical problem that the concrete industry has been continuously optimizing and solving. The existing methods for solving the segregation of concrete include adding inorganic dry powder to absorb moisture, adding organic or inorganic water-retaining agents, or adding viscosity enhancers. The above technical means all have certain limitations. They cannot deal with the encapsulation problem of concrete slurry well under the premise of a small amount of addition, and excessive addition will affect the strength of concrete. The existing anti-segregation agents have poor adaptability to aggregates. Once the quality of aggregates is poor, they cannot solve the segregation problem of concrete well. Especially for the segregation phenomenon of concrete mixtures with dry gneiss machine-made sand, the above technical means cannot solve the segregation phenomenon of concrete mixtures with gneiss machine-made sand 2 hours after discharge. Summary of the invention

[0003] The main purpose of the present invention is to develop an anti-segregation agent, which can well improve the encapsulation problem of concrete slurry on aggregate, especially inferior machine-made sand, and can prevent the concrete mixture from segregating after a long time of discharging without affecting the working performance of the concrete and keeping low cost.

[0004] To achieve the above-mentioned purpose, the present invention proposes an anti-segregation agent, which includes a dispersant, a thickener and a preservative; the dispersant includes a copolymer obtained by reaction monomers under the action of an initiator; the reaction monomers include an unsaturated carboxylic acid monomer and a first monomer; wherein the first monomer includes at least one of a sulfonic acid monomer, a silicone monomer, an aromatic monomer and a phosphate ester monomer.

[0005] In one embodiment, the reactive monomers include unsaturated carboxylic acid monomers and sulfonic acid monomers, silicone monomers, aromatic monomers, and phosphate monomers, and the weight ratio of the unsaturated carboxylic acid monomers, sulfonic acid monomers, silicone monomers, aromatic monomers, and phosphate monomers is (200-380): (0.5-1): (10-18): (20-30): (2-5).

[0006] In one embodiment, among the reaction monomers, the unsaturated carboxylic acid monomer includes at least one of itaconic acid, methacrylic acid, maleic acid, maleic anhydride, fumaric acid, aconitic acid, fumaric acid, methyl fumaric acid, acrylic acid, angelic acid, crotonic acid, isocrotonic acid butenoic acid, and propylene tricarboxylic acid.

[0007] In one embodiment, among the reactive monomers, the sulfonic acid monomer includes at least one of sodium styrene sulfonate, sodium p-styrene sulfonate, sodium methacrylic acid sulfonate, sodium vinyl sulfonate, 2-acrylamido-2-methylpropane sulfonic acid, 2-sulfoethyl methacrylate, sulfopropyl acrylate, and sulfopropyl methacrylate.

[0008] In one embodiment, in the reactive monomers, the organosilicon monomer includes at least one of vinyl tri(β-methoxyethoxy)silane, vinyl triethoxysilane, vinyl trimethoxysilane, vinyl triisopropoxysiloxane, and vinyl tri(2-methoxyethoxy)silane.

[0009] In one embodiment, among the reactive monomers, the aromatic monomer includes at least one of 2-phenoxyethyl acrylate and diethylene glycol phthalate diacrylate.

[0010] In one embodiment, among the reactive monomers, the phosphate monomer includes at least one of methacrylate phosphate and 2-hydroxyethyl methacrylate phosphate.

[0011] In one embodiment, the reactive monomer further comprises a second monomer, which is a functional monomer, and the functional monomer comprises at least one of methoxy polyethylene glycol (meth) acrylate, poly (ethylene glycol) methacrylate, tetradecyl acrylate, hexadecyl acrylate, and poly (ethylene glycol) methyl ether methacrylate.

[0012] In one embodiment, in the reaction monomers, the weight ratio of the unsaturated carboxylic acid monomer, the sulfonic acid monomer, the silicone monomer, the aromatic monomer, the phosphate monomer and the functional monomer is (200-380): (0.5-1): (10-18): (20-30): (2-5): (40-50).

[0013] In one embodiment, the dispersant includes the following raw materials in parts by weight: reaction monomer: 232.5 to 484 parts; initiator: 6 to 8 parts; hydrogen peroxide: 0.3 to 0.6 parts; sodium hydroxide: 180 to 220 parts; reducing agent: 12 to 27 parts; water: 770 to 980 parts.

[0014] In one embodiment, among the raw materials of the dispersant, the reducing agent includes at least one of sodium phosphite, sodium hypophosphite, bleaching powder, E51 reducing agent, sodium pyrosulfite, ferrous pyrophosphate, sodium thiosulfate, sodium bisulfite, sodium sulfite, potassium sulfite, sodium thiosulfate, tartaric acid, bleaching powder, ferrous sulfate, ferrous chloride, sodium hexametaphosphate, and vitamin C.

[0015] In one embodiment, in the raw materials of the dispersant, the initiator includes at least one of sodium persulfate, potassium persulfate, ammonium persulfate, hydrogen peroxide, tert-butyl hydroperoxide, cyclohexanone peroxide, and an azo initiator.

[0016] In one embodiment, in the anti-segregation agent, the weight ratio of the dispersant, thickener and preservative is 20:(10-13):(10-12).

[0017] In one embodiment, in the anti-segregation agent, the thickener includes at least one of guar gum, xanthan gum, vinasse, tapioca gum, potato gum, carrageenan, dextrin, and titanium dioxide.

[0018] In one embodiment, in the anti-segregation agent, the preservative includes at least one of isothiazolinone, 2-benzisothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, isoflavones, myricetin, 5,7-dihydroxyflavone, and soybean flavonoids.

[0019] In one embodiment, in the anti-segregation agent, the thickener comprises the following raw materials in parts by weight:

[0020] Hydroxypropyl guar gum with an average viscosity of 1500: 50-60 parts; Hydroxypropyl guar gum with an average viscosity of 4000: 30-40 parts; Xanthan gum: 6-10 parts; Wenlun gum: 5-8 parts.

[0021] In one embodiment, in the anti-segregation agent, the preservative comprises the following raw materials in parts by weight:

[0022] Isothiazolinone: 3-6 parts; 2-benzisothiazolin-3-one: 1-3 parts; 2-methyl-4-isothiazolin-3-one: 3-5 parts; isoflavone: 8-10 parts; water: 5-10 parts.

[0023] The present invention also provides a method for preparing the anti-segregation agent, characterized in that the method for preparing the anti-segregation agent comprises the following steps:

[0024] S10, adding the reaction monomer into a reaction container, adding an initiator, reacting, and preparing a dispersant;

[0025] S20, adding a thickener and a preservative into another reaction container and mixing, adding the dispersant prepared in step S10, stirring and mixing, and preparing the anti-segregation agent.

[0026] In one embodiment, the S10 specifically includes the following steps:

[0027] S101, add 90-130 parts of water and 6-8 parts of initiator to a reaction container, stir to dissolve, add 0.5-1 parts of sulfonic acid monomer and 120-150 parts of unsaturated carboxylic acid monomer, stir to mix, add 10-18 parts of organosilicon monomer, stir to mix, and prepare liquid A;

[0028] S102, adding 50-60 parts of water, 2-5 parts of phosphate monomers and 20-30 parts of aromatic monomers into a reaction container, stirring and mixing, to obtain liquid B;

[0029] S103, adding 50-60 parts of water and 40-50 parts of functional monomers into a reaction container, stirring and mixing, to obtain liquid C;

[0030] S104, adding 280-330 parts of water into a reaction container, and gradually and slowly adding a total amount of 180-220 parts of sodium hydroxide to obtain a D solution;

[0031] S105, adding 350-400 parts of water and 200-230 parts of unsaturated carboxylic acid monomer into a reaction container, stirring to dissolve, and dripping the D solution prepared in the step S104, performing the first dripping of D solution, with the dripping of D solution, the temperature of the reaction system rises, when the temperature rises to 60-65°C, stopping the dripping of D solution, adding 12-27 parts of reducing agent and 0.3-0.6 parts of hydrogen peroxide and keeping the temperature for reaction for 20 minutes, after the reaction is completed, removing the heat source and dripping A solution, starting to drip B solution 30 minutes after the start of dripping A solution, starting to drip C solution 70 minutes after the start of dripping A solution, adding the remaining D solution 20 minutes after the completion of dripping C solution, performing the second dripping of D solution, and completing all reactions to obtain the dispersant.

[0032] In one embodiment, in step S105, when the D solution is dripped for the first time, the dripping rate is controlled to be 120 portions per hour;

[0033] In the step S105, when the liquid A is dripped, the total dripping time is controlled to be 120 minutes, and 65% of the total amount of the liquid A is dripped in the first half of the total dripping time, and the temperature of the reaction system is controlled at 50-70° C. during the dripping process;

[0034] In the step S105, when the B solution is added dropwise, the total addition time of the B solution is controlled to be 60 minutes;

[0035] In the step S105, when the C solution is added dropwise, the total addition time of the C solution is controlled to be 60 minutes;

[0036] In the step S105, when the D solution is dripped for the second time, the temperature of the reaction system is controlled at 70-85°C during the dripping process, and the total time of the first and second dripping of the D solution does not exceed 150 minutes.

[0037] In one implementation, the step S20 specifically includes the following steps:

[0038] S201, adding 50-60 parts of hydroxypropyl guar gum with an average viscosity of 1500, 30-40 parts of hydroxypropyl guar gum with an average viscosity of 4000, 6-10 parts of xanthan gum and 5-8 parts of vinblastine gum into a reaction container, stirring and mixing to prepare a thickener;

[0039] S202, adding 3 to 6 parts of isothiazolinone, 1 to 3 parts of 2-benzisothiazolin-3-one, 3 to 5 parts of 2-methyl-4-isothiazolin-3-one, 8 to 10 parts of isoflavones and 5 to 10 parts of water into a reaction container, stirring and mixing to obtain a preservative;

[0040] S203, adding 10 to 13 parts of the thickener prepared in step S201, 20 parts of the dispersant prepared in step S105 and 10 to 12 parts of the preservative prepared in step S202, and fixing the volume to 500 mL to prepare the anti-segregation agent.

[0041] The invention also proposes application of the anti-segregation agent in concrete slurry.

[0042] The technical solution of the present invention designs an anti-segregation agent, which synthesizes a dispersant with low molecular weight and strong dispersibility by selecting specific reactive monomers with different functions such as sulfonic acid monomers, silicone monomers, aromatic monomers and phosphate monomers to be grafted onto the polymer main chain formed by unsaturated carboxylic acids, which can well improve the encapsulation problem of concrete slurry on aggregates, especially inferior machine-made sand; the dispersant is used as the main component, and the dispersant is mixed with a plant-based thickener to achieve a modified treatment of the thickener, and the product is applied to the concrete slurry to further improve the suspension and encapsulation of the concrete slurry; in addition, a preservative with a specific formula is added to the anti-segregation agent, which can further improve the anti-flocculation performance of the concrete slurry. The anti-segregation agent in the present invention has a wider range of adaptability to concrete aggregates, a larger upper and lower limit range of concrete segregation state, a stronger ability to adjust concrete mixtures, a more flexible way of adding and using, and a lower production cost. DETAILED DESCRIPTION

[0043] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0044] It should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back, etc.), the directional indications are only used to explain the relative position relationship, movement status, etc. between the components in a certain specific posture. If the specific posture changes, the directional indication will also change accordingly.

[0045] In addition, if there are descriptions involving "first", "second", etc. in the embodiments of the present invention, the descriptions of "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of technical features indicated. Therefore, the features limited to "first" and "second" may explicitly or implicitly include at least one of the features. In addition, if "and / or" or "and / or" appears in the full text, its meaning includes three parallel solutions. Taking "A and / or B" as an example, it includes solution A, solution B, or solutions that satisfy both A and B. In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the ability of ordinary technicians in this field to implement. When the combination of technical solutions is contradictory or cannot be implemented, it should be deemed that such combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0046] The technical problem solved by the present invention is the segregation problem of concrete mixtures. The technical means in the prior art have certain limitations. They cannot well deal with the encapsulation problem of concrete slurry under the premise of a small amount of addition, and excessive addition will affect the strength of concrete. The existing anti-segregation agent has poor adaptability to aggregates. Once the quality of the aggregate is poor, it cannot well solve the segregation problem of concrete. In particular, for the segregation phenomenon of concrete mixtures with dry gneiss machine-made sand, the above technical means cannot solve the segregation phenomenon of concrete mixtures with gneiss machine-made sand 2 hours after discharge.

[0047] In order to solve the above technical problems, an anti-segregation agent is designed, which can effectively improve the encapsulation of concrete slurry on aggregate, especially inferior machine-made sand, and can prevent the concrete mixture from segregating after a long time of discharging without affecting the working performance of concrete and keeping low cost.

[0048] The present invention provides an anti-segregation agent, which includes a dispersant, a thickener and a preservative; the dispersant includes a copolymer obtained by reacting monomers under the action of an initiator; the reacting monomers include an unsaturated carboxylic acid monomer and a first monomer; wherein the first monomer includes at least one of a sulfonic acid monomer, an organosilicon monomer, an aromatic monomer and a phosphate ester monomer.

[0049] It should be noted that the anti-segregation agent in the present invention uses a dispersant with special functional monomers as the main material of the anti-segregation agent. The dispersant has the advantages of low molecular weight and high adsorption, with a carbon chain formed by copolymerization of unsaturated carboxylic acid monomers as the main chain, and a specific proportion of monomers with specific functional groups such as sulfonic acid monomers, silicone monomers, aromatic monomers and phosphate monomers are selected to be grafted onto the main chain through copolymerization, so that the prepared dispersant has strong dispersibility, good water retention and good wrapping of concrete aggregates; the thickener is mainly used to increase the viscosity of the concrete slurry and change the rheological properties of the concrete to reduce the segregation phenomenon.

[0050] In one embodiment, the reactive monomers include unsaturated carboxylic acid monomers and sulfonic acid monomers, silicone monomers, aromatic monomers, and phosphate monomers, and the weight ratio of the unsaturated carboxylic acid monomers, sulfonic acid monomers, silicone monomers, aromatic monomers, and phosphate monomers is (200-380): (0.5-1): (10-18): (20-30): (2-5). It should be noted that among the unsaturated carboxylic acid monomers, the weight ratio of the monomer used as the main chain to the monomer used as the branch chain is (200-230): (0-150); the sulfonic acid monomers, silicone monomers, aromatic monomers, and phosphate monomers are all used as reactive monomers on the branch chains.

[0051] It should also be noted that by reasonably controlling the types and ratios of the reactive monomers on the main chain and the side chains, the molecular weight of the prepared dispersant is made smaller and the hydrophilicity is stronger, thereby making the prepared dispersant have stronger dispersibility; the molecular weight of the dispersant in the present invention is between 1500 and 8000.

[0052] In one embodiment, among the reaction monomers, the unsaturated carboxylic acid monomer includes at least one of itaconic acid, methacrylic acid, maleic acid, maleic anhydride, fumaric acid, aconitic acid, fumaric acid, methyl fumaric acid, acrylic acid, angelic acid, crotonic acid, isocrotonic acid butenoic acid, and propylene tricarboxylic acid.

[0053] In one embodiment, among the reactive monomers, the sulfonic acid monomer includes at least one of sodium styrene sulfonate, sodium p-styrene sulfonate, sodium methacrylic acid sulfonate, sodium vinyl sulfonate, 2-acrylamido-2-methylpropane sulfonic acid, 2-sulfoethyl methacrylate, sulfopropyl acrylate, and sulfopropyl methacrylate.

[0054] In one embodiment, in the reactive monomers, the organosilicon monomer includes at least one of vinyl tri(β-methoxyethoxy)silane, vinyl triethoxysilane, vinyl trimethoxysilane, vinyl triisopropoxysiloxane, and vinyl tri(2-methoxyethoxy)silane.

[0055] In one embodiment, among the reactive monomers, the aromatic monomer includes at least one of 2-phenoxyethyl acrylate and diethylene glycol phthalate diacrylate.

[0056] In one embodiment, among the reactive monomers, the phosphate monomer includes at least one of methacrylate phosphate and 2-hydroxyethyl methacrylate phosphate.

[0057] It should be noted that sulfonic acid monomers are introduced into the dispersant side chains. The sulfonic acid groups in the sulfonic acid monomers have good water solubility. The sulfonic acid groups can be completely dissociated in aqueous solution to form corresponding salts with cations, which can release water molecules adsorbed by hydrated cations in the slurry, thereby reducing the viscosity of the slurry and making it less prone to thixotropy; silicone monomers are introduced into the dispersant side chains. The silicon-oxygen bonds in the silicone monomers can increase the crosslinking degree and stability of the dispersant, increase the glass transition temperature of the material, thereby improving its heat resistance, thereby improving the dispersant's encapsulation and durability of concrete aggregates, and significantly improving the appearance color and uniformity of concrete; aromatic monomers are introduced into the dispersant side chains. The benzene rings in the aromatic monomers increase the spatial repulsion of the dispersant in the concrete mixture and thus improve the dispersibility and mud resistance; phosphate ester monomers are introduced into the dispersant side chains. The phosphate groups in the phosphate ester monomers have good hydrophilicity and water retention. On the one hand, they can improve the fluidity of the concrete mixture, and on the other hand, they can regulate the early hydration reaction of the concrete, thereby improving the uniformity and mud resistance of the concrete.

[0058] It should also be noted that the reactive monomers constituting the dispersant in the present invention can only participate in the polymerization reaction in the form of an acid, but cannot participate in the copolymerization reaction in the form of a salt. This is because the pH value of the copolymer, i.e. the dispersant, generated after participating in the copolymerization reaction in the form of an acid is 3 to 6. In the subsequent mixing process of the dispersant and the plant gum thickener, the acidic dispersant has a modifying effect on the plant gum thickener, and can hydrolyze the high molecular weight thickener into a low molecular weight one, thereby maintaining the molecular weight of the obtained anti-segregation agent at about 1500 to 8000, so that the obtained anti-segregation agent can be better dispersed in the concrete slurry.

[0059] In one embodiment, the reaction monomer further comprises a second monomer, which is a functional monomer, and the functional monomer comprises at least one of methoxy polyethylene glycol (meth) acrylate, poly (ethylene glycol) methacrylate, tetradecyl acrylate, hexadecyl acrylate, and poly (ethylene glycol) methyl ether methacrylate. It should be noted that the methoxy polyethylene glycol (meth) acrylate, poly (ethylene glycol) methacrylate, and poly (ethylene glycol) methyl ether methacrylate in the functional monomers of the present invention are all low molecular weight functional monomers; preferably, the molecular weight of the methoxy polyethylene glycol (meth) acrylate is 900 to 1200; preferably, the molecular weight of the poly (ethylene glycol) methacrylate is 900 to 1200; preferably, the molecular weight of the poly (ethylene glycol) methyl ether methacrylate is 900 to 1200.

[0060] It should also be noted that in the present invention, functional monomers are introduced into the dispersant side chains, and the functional monomers are low molecular weight functional monomers, which can ensure that the copolymer formed by the copolymerization reaction has a smaller molecular weight and thus ensure its dispersibility. In addition, the copolymerization reaction can reach the reaction temperature and continue to react completely without an external heat source according to the designed reaction system, so that the preparation of the dispersant in the present invention does not rely on external experimental facilities, further reducing production costs.

[0061] In one embodiment, among the reactive monomers, the weight ratio of the unsaturated carboxylic acid monomer, the sulfonic acid monomer, the organosilicon monomer, the aromatic monomer, the phosphate ester monomer and the functional monomer is (200-380): (0.5-1): (10-18): (20-30): (2-5): (40-50). It should be noted that among the unsaturated carboxylic acid monomers, the weight ratio of the monomer used as the main chain to the monomer used as the branch chain is (200-230): (0-150); the sulfonic acid monomer, the organosilicon monomer, the aromatic monomer, the phosphate ester monomer and the functional monomer are all used as reactive monomers on the branch chain.

[0062] It should also be noted that by reasonably controlling the types and ratios of the reactive monomers on the main chain and the side chains, the molecular weight of the prepared dispersant is made smaller and the hydrophilicity is stronger, thereby making the prepared dispersant have stronger dispersibility; the molecular weight of the dispersant in the present invention is between 1500 and 8000.

[0063] In one embodiment, the dispersant includes the following raw materials in parts by weight: reaction monomer: 232.5-484 parts; initiator: 6-8 parts; hydrogen peroxide: 0.3-0.6 parts; sodium hydroxide: 180-220 parts; reducing agent: 12-27 parts; water: 770-980 parts.

[0064] It should be noted that, in this embodiment, sodium hydroxide is used to increase the reaction rate of the copolymerization reaction, and the initiator and a trace amount of hydrogen peroxide can initiate a free radical polymerization reaction.

[0065] In one embodiment, among the raw materials of the dispersant, the reducing agent includes at least one of sodium phosphite, sodium hypophosphite, bleaching powder, E51 reducing agent, sodium pyrosulfite, ferrous pyrophosphate, sodium thiosulfate, sodium bisulfite, sodium sulfite, potassium sulfite, sodium thiosulfate, tartaric acid, bleaching powder, ferrous sulfate, ferrous chloride, sodium hexametaphosphate, and vitamin C.

[0066] In one embodiment, in the raw materials of the dispersant, the initiator includes at least one of sodium persulfate, potassium persulfate, ammonium persulfate, hydrogen peroxide, tert-butyl hydroperoxide, cyclohexanone peroxide, and an azo initiator.

[0067] In one embodiment, in the anti-segregation agent, the weight ratio of the dispersant, thickener and preservative is 20:(10-13):(10-12).

[0068] In one embodiment, in the anti-segregation agent, the thickener includes at least one of hydroxypropyl guar gum, guar gum, xanthan gum, vinyl gum, sodium hydroxymethyl cellulose, tapioca gum, potato gum, carrageenan, dextrin, and titanium dioxide. It should be noted that the thickeners are all plant-based thickeners, which can be self-degraded and will not produce any pollutants. At the same time, plant-based thickeners are easily modified, so that the proportion of the anti-segregation agent can be adjusted according to the properties of the concrete aggregate.

[0069] In one embodiment, the hydroxypropyl guar gum includes nonionic hydroxypropyl guar gum with an average viscosity of 1500 cps and anionic hydroxypropyl guar gum with an average viscosity of 4000 cps. In this embodiment, by compounding two hydroxypropyl guar gums with different viscosities, the viscosity adjustment range of the prepared thickener is wider.

[0070] In one embodiment, the preservative includes at least one of isothiazolinone, 2-benzisothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, isoflavone, myricetin, 5,7-dihydroxyflavone, and soybean flavonoids. It should be noted that in addition to its own antioxidant, bactericidal, antiseptic, and stabilizer functions, the preservative in this embodiment also has the function of reducing the adverse effects of the polyacrylamide flocculant remaining in the washed sand on the concrete mixture, and has an anti-flocculation effect.

[0071] In one embodiment, in the anti-segregation agent, the thickener includes the following raw materials in parts by weight: non-ionic hydroxypropyl guar gum with an average viscosity of 1500cps: 50-60 parts; anionic hydroxypropyl guar gum with an average viscosity of 4000cps: 30-40 parts; xanthan gum: 6-10 parts; and wenlun gum: 5-8 parts. It should be noted that the thickener using the above formula can better match the dispersant, and the anti-segregation agent obtained after blending with the dispersant has better encapsulation of concrete aggregates.

[0072] In one embodiment, in the anti-segregation agent, the preservative includes the following raw materials in parts by weight: isothiazolinone: 3 to 6 parts; 2-benzisothiazolin-3-one: 1 to 3 parts; 2-methyl-4-isothiazolin-3-one: 3 to 5 parts; isoflavone: 8 to 10 parts; water: 5 to 10 parts. It should be noted that the preservative using the above formula can effectively prevent the formation of slime by killing the sludge-forming bacteria in the concrete slurry, and has a certain anti-flocculation effect.

[0073] The present invention also provides a method for preparing the anti-segregation agent, which specifically comprises the following steps:

[0074] S10, adding the reaction monomer into a reaction container, adding an initiator, reacting, and preparing a dispersant;

[0075] S20, adding a thickener and a preservative into another reaction container and mixing, adding the dispersant prepared in step S10, stirring and mixing, and preparing the anti-segregation agent.

[0076] In one embodiment, the S10 specifically includes the following steps:

[0077] S101, add 90-130 parts of water and 6-8 parts of initiator to a reaction container, stir to dissolve, add 0.5-1 parts of sulfonic acid monomer and 120-150 parts of unsaturated carboxylic acid monomer, stir to mix, add 10-18 parts of organosilicon monomer, stir to mix, and prepare liquid A;

[0078] S102, adding 50-60 parts of water, 2-5 parts of phosphate monomers and 20-30 parts of aromatic monomers into a reaction container, stirring and mixing, to obtain liquid B;

[0079] S103, adding 50-60 parts of water and 40-50 parts of functional monomers into a reaction container, stirring and mixing, to obtain liquid C;

[0080] S104, adding 280-330 parts of water into a reaction container, and gradually and slowly adding a total amount of 180-220 parts of sodium hydroxide to obtain a D solution;

[0081] S105, adding 350-400 parts of water and 200-230 parts of unsaturated carboxylic acid monomer into a reaction container, stirring to dissolve, and dripping the D solution prepared in the step S104, performing the first dripping of D solution, with the dripping of D solution, the temperature of the reaction system rises, when the temperature rises to 60-65°C, stopping the dripping of D solution, adding 12-27 parts of reducing agent and 0.3-0.6 parts of hydrogen peroxide and keeping the temperature for reaction for 20 minutes, after the reaction is completed, removing the heat source and dripping A solution, starting to drip B solution 30 minutes after the start of dripping A solution, starting to drip C solution 70 minutes after the start of dripping A solution, adding the remaining D solution 20 minutes after the completion of dripping C solution, performing the second dripping of D solution, and completing all reactions to obtain the dispersant.

[0082] In one embodiment, in step S105, when the D solution is dripped for the first time, the dripping rate is controlled to be 120 portions per hour;

[0083] In the step S105, when the liquid A is dripped, the total dripping time is controlled to be 120 minutes, and 65% of the total amount of the liquid A is dripped in the first half of the total dripping time, and the temperature of the reaction system is controlled at 50-70° C. during the dripping process;

[0084] In the step S105, when the B solution is added dropwise, the total addition time of the B solution is controlled to be 60 minutes;

[0085] In the step S105, when the C solution is added dropwise, the total addition time of the C solution is controlled to be 60 minutes;

[0086] In the step S105, when the D solution is dripped for the second time, the temperature of the reaction system is controlled at 70-85°C during the dripping process, and the total time of the first and second dripping of the D solution does not exceed 150 minutes.

[0087] It should be noted that in this embodiment, the specific reaction steps in the preparation method of the anti-segregation agent and the specific component ratios in each step are precisely combined to rationally control the types and ratios of specific functional groups on the main chain and side chains of the dispersant, so that the comprehensive performance of the dispersant as the main material of the anti-segregation agent is stronger.

[0088] In one embodiment, the step S20 specifically includes the following steps:

[0089] S201, adding 50-60 parts of nonionic hydroxypropyl guar gum with an average viscosity of 1500, 30-40 parts of anionic hydroxypropyl guar gum with an average viscosity of 4000, 6-10 parts of xanthan gum and 5-8 parts of vinblastine gum into a reaction container, stirring and mixing to prepare a thickener;

[0090] S202, adding 3 to 6 parts of isothiazolinone, 1 to 3 parts of 2-benzisothiazolin-3-one, 3 to 5 parts of 2-methyl-4-isothiazolin-3-one, 8 to 10 parts of isoflavones and 5 to 10 parts of water into a reaction container, stirring and mixing to obtain a preservative;

[0091] S203, adding 10 to 13 parts of the thickener prepared in step S201, 20 parts of the dispersant prepared in step S105 and 10 to 12 parts of the preservative prepared in step S202, and fixing the volume to 500 mL to prepare the anti-segregation agent.

[0092] It should be noted that, in this embodiment, by blending and modifying the dispersant and the plant-based thickener, and adding a specific formula preservative, the advantages of different anti-segregation systems in the anti-segregation agent can be maximized, so that the anti-segregation agent in the present invention has a wider range of adaptability to concrete aggregates, a larger upper and lower limit range of concrete segregation state, a stronger ability to adjust concrete mixtures, a more flexible way of adding and using, and a lower production cost.

[0093] In one embodiment, in the step S20, after the dispersant with a pH value less than 3 is mixed with the thickener and the preservative, the thickener with a large molecular weight can be hydrolyzed into a thickener with a small molecular weight. The anti-segregation agent obtained in this case can effectively reduce the overall viscosity of the prepared anti-segregation agent, and the anti-segregation agent has better suspension performance when added to the concrete mixture. In one embodiment, water is added to the thickener to change it from a dry powder to a liquid, and then mixed with the dispersant and the preservative, so that the anti-segregation agent takes effect faster.

[0094] The invention also proposes application of the anti-segregation agent in concrete slurry.

[0095] It should be noted that the anti-segregation agent in the present invention is used in the concrete mixture of dry gneiss machine-made sand, and no serious segregation will occur after discharging for 2 hours or longer; the anti-segregation agent in the present invention has a wider upper and lower limit adjustment range for the concrete state, and the addition method and use method are more flexible, which can improve the comprehensive performance of concrete more comprehensively and have lower production costs.

[0096] The present invention is further described below by means of specific embodiments:

[0097] The sources of the raw materials used in the examples of the present invention are all commercially available, and the present invention does not impose any special restrictions on the sources of the raw materials.

[0098] Nonionic hydroxypropyl guar gum with an average viscosity of 1500 cps was purchased from Zhengzhou Yufan Biotechnology Co., Ltd.;

[0099] Anionic hydroxypropyl guar gum with an average viscosity of 4000 cps was purchased from Zhengzhou Yufan Biotechnology Co., Ltd.;

[0100] Xanthan gum was purchased from Zhengzhou Yufan Biotechnology Co., Ltd.;

[0101] Wenlunjiao was purchased from Zhengzhou Yufan Biotechnology Co., Ltd.;

[0102] Maleic acid was purchased from Tianjin Zhonglian Chemical Reagent Co., Ltd.; acrylic acid was purchased from Guangdong Shiboshi New Materials Co., Ltd.;

[0103] Sodium p-styrene sulfonate, purchased from Shandong Yousuo Chemical Technology Co., Ltd., content 99%;

[0104] Vinyl tri(β-methoxyethoxy)silane, purchased from Shandong Sodium Magnesium New Materials Co., Ltd.; Vinyl triethoxysilane: purchased from Shandong Yuanjin New Materials Co., Ltd.;

[0105] Methacrylate phosphate, purchased from Hubei Watson Chemical Technology Co., Ltd., purity 99%;

[0106] Ammonium persulfate: Wuhan Jiyesheng Chemical Co., Ltd.;

[0107] Hydrogen peroxide: purchased from Guangdong Shiboshi New Materials Co., Ltd.;

[0108] Sodium hydroxide: purchased from Jinan 168 Chemical Co., Ltd.

[0109] Sodium hypophosphite: purchased from Guangdong Guangye New Materials Co., Ltd.;

[0110] Bleaching agent: purchased from Shanghai APB Chemical Reagent Co., Ltd.

[0111] Isothiazolinone: purchased from Shandong Delan Chemical Co., Ltd.;

[0112] Benzisothiazoline-3-one: Wuhan Smik Biotechnology Co., Ltd.;

[0113] Methyl-4-isothiazolin-3-one: Wuhan Jiyesheng Chemical Co., Ltd.;

[0114] Isoflavones: Hebei Kelongduo Biotechnology Co., Ltd.

[0115] Examples 1 to 5

[0116] The anti-segregation agent in Examples 1 to 5 includes a dispersant, a thickener and a preservative;

[0117] Wherein, the dispersant comprises the following raw materials in parts by weight:

[0118] 200-230 parts of unsaturated carboxylic acid monomer, 0.5-1 parts of sulfonic acid monomer, 10-18 parts of silicone monomer, 2-5 parts of phosphate monomer, 20-30 parts of aromatic monomer, 6-8 parts of initiator, 0.3-0.6 parts of hydrogen peroxide, 180-220 parts of sodium hydroxide, 12-16 parts of reducing agent, and 770-920 parts of water.

[0119] Among them, in the dispersants of Examples 1 to 5, the unsaturated carboxylic acid monomer is maleic acid, the sulfonic acid monomer is sodium p-styrene sulfonate, the silicone monomer is vinyl tri(β-methoxyethoxy) silane, the phosphate ester monomer is methyl methacrylate phosphate, the aromatic monomer is 2-phenoxyethyl acrylate, the initiator is ammonium persulfate, and the reducing agent is sodium hypophosphite.

[0120] The specific raw material ratios of the dispersants of Examples 1 to 5 are shown in Table 1.

[0121] Table 1

[0122]

[0123] The formulas of thickener and preservative in Examples 1 to 5 are the same, specifically as follows:

[0124] The thickener includes: 50 parts of nonionic hydroxypropyl guar gum with an average viscosity of 1500, 40 parts of anionic hydroxypropyl guar gum with an average viscosity of 4000, 8 parts of xanthan gum, and 7 parts of vinblastine gum.

[0125] The preservatives include: 5 parts of isothiazolinone, 3 parts of 2-benzisothiazolin-3-one, 3 parts of 2-methyl-4-isothiazolin-3-one, 8 parts of isoflavones and 10 parts of water.

[0126] The preparation method of the anti-segregation agent in Examples 1 to 5 comprises the following steps:

[0127] S101, adding 100 parts of water and an initiator to a reaction container, stirring to dissolve, adding a sulfonic acid monomer and an unsaturated carboxylic acid monomer, stirring to mix, adding an organosilicon monomer, stirring to mix, and obtaining a liquid A;

[0128] S102, adding 50 parts of water, phosphate monomer and aromatic monomer into a reaction container, stirring and mixing, to obtain liquid B;

[0129] S104, adding 310 parts of water into the reaction container, and slowly adding sodium hydroxide in succession to obtain liquid D;

[0130] S105, add 360 parts of water and unsaturated carboxylic acid monomer to the reaction container, stir and dissolve, drop the D liquid prepared in step S104, and perform the first drop of D liquid. With the drop of D liquid, the temperature of the reaction system rises. When the temperature rises to 60-65°C, stop dropping D liquid, add reducing agent and hydrogen peroxide and keep warm for reaction for 20 minutes. After the reaction is completed, remove the heat source and drop A liquid. The total drop time is 120 minutes, and 65% is added in the first 60 minutes. During the drop of A liquid, the temperature is controlled within the range of 50-70°C. 30 minutes after the drop of A liquid begins, the drop of B liquid begins, and the total drop time of B liquid is 60 minutes. 20 minutes after the drop of B liquid is completed, the remaining D liquid is added, and the second drop of D liquid is performed. During the drop of D liquid, the temperature of the reaction system is controlled within the range of 70-85°C. The total time of the first and second drop of D liquid does not exceed 150 minutes. After all the reactions are completed, the dispersant is obtained.

[0131] S201, adding nonionic hydroxypropyl guar gum with an average viscosity of 1500, anionic hydroxypropyl guar gum with an average viscosity of 4000, xanthan gum and guar gum into a reaction container, stirring and mixing to prepare a thickener;

[0132] S202, adding isothiazolinone, 2-benzisothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, isoflavone and water into a reaction container, stirring and mixing to obtain a preservative;

[0133] S203, adding water to 12 parts of the thickener prepared in step S201, 20 parts of the dispersant prepared in step S105 and 12 parts of the preservative prepared in step S202 to make the volume to 500 mL, to prepare the anti-segregation agent.

[0134] Embodiments 6 to 10

[0135] The anti-segregation agent in Examples 6 to 10 includes a dispersant, a thickener and a preservative;

[0136] Wherein, the dispersant comprises the following raw materials in parts by weight:

[0137] 320-380 parts of unsaturated carboxylic acid monomer, 0.5-1 parts of sulfonic acid monomer, 10-18 parts of silicone monomer, 2-5 parts of phosphate monomer, 20-30 parts of aromatic monomer, 40-50 parts of functional monomer, 6-8 parts of initiator, 0.3-0.6 parts of hydrogen peroxide, 180-220 parts of sodium hydroxide, 12-27 parts of reducing agent, and 820-980 parts of water.

[0138] Among them, in the dispersants of Examples 1 to 5, the unsaturated carboxylic acid monomer uses maleic acid and acrylic acid in a weight ratio of (200 to 230): (120 to 150), the sulfonic acid monomer uses sodium p-styrene sulfonate, the silicone monomer uses vinyl tri(β-methoxyethoxy) silane, the phosphate ester monomer uses methyl methacrylate phosphate, the aromatic monomer uses 2-phenoxyethyl acrylate, the functional monomer uses methoxy polyethylene glycol (meth) acrylate with a molecular weight of 900 to 1200, the initiator uses ammonium persulfate, and the reducing agent uses a mixture of sodium hypophosphite, bleaching powder and vitamins in a weight ratio of 12:5:3.

[0139] The specific raw material ratios of the dispersants of Examples 6 to 10 are shown in Table 2.

[0140] Table 2

[0141]

[0142]

[0143] The formulas of thickener and preservative in Examples 6 to 10 are the same, specifically as follows:

[0144] The thickener includes: 50 parts of nonionic hydroxypropyl guar gum with an average viscosity of 1500, 40 parts of anionic hydroxypropyl guar gum with an average viscosity of 4000, 8 parts of xanthan gum, and 7 parts of vinblastine gum.

[0145] The preservatives include: 5 parts of isothiazolinone, 3 parts of 2-benzisothiazolin-3-one, 3 parts of 2-methyl-4-isothiazolin-3-one, 8 parts of isoflavones and 10 parts of water.

[0146] The preparation method of the anti-segregation agent in Examples 6 to 10 comprises the following steps:

[0147] S101, adding an initiator and 100 parts of water into a reaction container, stirring to dissolve, adding a sulfonic acid monomer and acrylic acid, stirring to mix, adding an organosilicon monomer, stirring to mix, and obtaining a liquid A;

[0148] S102, adding phosphate monomer, aromatic monomer and 50 parts of water into a reaction container, stirring and mixing, to obtain liquid B;

[0149] S103, adding functional monomers and 50 parts of water into a reaction container, stirring and mixing, to obtain liquid C;

[0150] S104, adding 310 parts of water into the reaction container, and slowly adding sodium hydroxide in succession to obtain liquid D;

[0151] S105, adding maleic acid and 360 parts of water into a reaction container, stirring to dissolve, and dripping the D solution prepared in step S104, performing the first dripping of D solution. With the dripping of D solution, the temperature of the reaction system rises. When the temperature rises to 60-65°C, stop dripping D solution, add a reducing agent and hydrogen peroxide and keep the temperature for reaction for 20 minutes. After the reaction is completed, remove the heat source and drip A solution. The total dripping time of A solution is 120 minutes, and 65% is dripped in the first 60 minutes. During the dripping process of A solution, the temperature is controlled in the range of 50-70°C. Liquid B was added 30 minutes after the start of the dropwise addition of liquid A, and liquid C was added 70 minutes after the start of the dropwise addition of liquid A. The total dropwise addition time of liquid B was 60 minutes, and the total dropwise addition time of liquid C was 60 minutes. 20 minutes after the dropwise addition of liquid C was completed, the remaining liquid D was added dropwise, and liquid D was added dropwise for the second time. During the second dropwise addition of liquid D, the temperature of the reaction system was controlled within the range of 70 to 85° C., and the total time for the first and second dropwise additions of liquid D did not exceed 150 minutes. After all the reactions were completed, the dispersant was obtained.

[0152] S201, adding nonionic hydroxypropyl guar gum with an average viscosity of 1500, anionic hydroxypropyl guar gum with an average viscosity of 4000, xanthan gum and guar gum into a reaction container, stirring and mixing to prepare a thickener;

[0153] S202, adding isothiazolinone, 2-benzisothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, isoflavone and water into a reaction container, stirring and mixing to obtain a preservative;

[0154] S203, adding water to 12 parts of the thickener prepared in step S201, 20 parts of the dispersant prepared in step S105 and 12 parts of the preservative prepared in step S202 to make the volume to 500 mL, to prepare the anti-segregation agent.

[0155] Comparative Example 1

[0156] The anti-segregation agent in Comparative Example 1 includes a dispersant, a thickener and a preservative;

[0157] Wherein, the dispersant comprises the following raw materials in parts by weight:

[0158] 370 parts of unsaturated carboxylic acid monomer, 8 parts of initiator, 0.5 parts of hydrogen peroxide, 200 parts of sodium hydroxide, 15 parts of reducing agent, and 770 parts of water.

[0159] In the dispersant of Comparative Example 1, the unsaturated carboxylic acid monomer includes 220 parts of maleic acid and 150 parts of acrylic acid, the initiator is ammonium persulfate, and the reducing agent is sodium hypophosphite.

[0160] The formula of thickener and preservative in Comparative Example 1 is the same as that in Example 1.

[0161] The preparation method of the anti-segregation agent in Comparative Example 1 comprises the following steps:

[0162] S101, adding an initiator and 100 parts of water into a reaction container, stirring to dissolve, adding acrylic acid, stirring to mix, to obtain liquid A;

[0163] S104, adding 310 parts of water into the reaction container, and slowly adding sodium hydroxide in succession to obtain liquid D;

[0164] S105, add maleic acid and 360 parts of water to the reaction container, stir and dissolve, dropwise add the D solution prepared in step S104, perform the first dropwise addition of D solution, with the dropwise addition of D solution, the temperature of the reaction system rises, when the temperature rises to 60-65°C, stop dropping D solution, add reducing agent and hydrogen peroxide and keep warm for reaction for 20 minutes, after the reaction is completed, remove the heat source and dropwise add A solution, the total dropwise addition time of A solution is 120 minutes, 65% is added in the first 60 minutes; during the dropwise addition of A solution, the temperature is controlled within the range of 50-70°C. 20 minutes after the dropwise addition of A solution is completed, dropwise add the remaining D solution, perform the second dropwise addition of D solution, during the second dropwise addition of D solution, the temperature of the reaction system is controlled within the range of 70-85°C, the total time of the first and second dropwise additions of D solution does not exceed 150 minutes; after all reactions are completed, the dispersant is obtained.

[0165] S201, adding nonionic hydroxypropyl guar gum with an average viscosity of 1500, anionic hydroxypropyl guar gum with an average viscosity of 4000, xanthan gum and guar gum into a reaction container, stirring and mixing to prepare a thickener;

[0166] S202, adding isothiazolinone, 2-benzisothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, isoflavone and water into a reaction container, stirring and mixing to obtain a preservative;

[0167] S203, adding water to 12 parts of the thickener prepared in step S201, 20 parts of the dispersant prepared in step S105 and 12 parts of the preservative prepared in step S202 to make the volume to 500 mL, to prepare the anti-segregation agent.

[0168] Comparative Example 2

[0169] The anti-segregation agent in Comparative Example 2 includes a dispersant, a thickener and a preservative;

[0170] Wherein, the dispersant comprises the following raw materials in parts by weight (same as in Example 7):

[0171] 370 parts of unsaturated carboxylic acid monomer, 0.8 parts of sulfonic acid monomer, 14 parts of silicone monomer, 3 parts of phosphate monomer, 25 parts of aromatic monomer, 40 parts of functional monomer, 8 parts of initiator, 0.5 parts of hydrogen peroxide, 200 parts of sodium hydroxide, 20 parts of reducing agent, and 870 parts of water.

[0172] Among them, in the dispersant of Comparative Example 2, the unsaturated carboxylic acid monomer includes 220 parts of maleic acid and 150 parts of acrylic acid, the sulfonic acid monomer adopts sodium p-styrene sulfonate, the silicone monomer adopts vinyl tri(β-methoxyethoxy) silane, the phosphate monomer adopts methyl methacrylate phosphate, the aromatic monomer adopts 2-phenoxyethyl acrylate, the functional monomer adopts methoxy polyethylene glycol (methyl) acrylate with a molecular weight of 900 to 1200, the initiator adopts ammonium persulfate, and the reducing agent adopts a mixture of sodium hypophosphite, bleaching powder and vitamins in a weight ratio of 12:5:3.

[0173] The formula and preparation method of the thickener and preservative in Comparative Example 2 are the same as those in Example 7.

[0174] The preparation method of the anti-segregation agent in Comparative Example 2 comprises the following steps:

[0175] S101, adding an initiator and 100 parts of water into a reaction container, stirring to dissolve, adding a sulfonic acid monomer and acrylic acid, stirring to mix, adding an organosilicon monomer, stirring to mix, and obtaining a liquid A;

[0176] S102, adding phosphate monomer, aromatic monomer and 50 parts of water into a reaction container, stirring and mixing, to obtain liquid B;

[0177] S103, adding functional monomers and 50 parts of water into a reaction container, stirring and mixing, to obtain liquid C;

[0178] S104, adding 310 parts of water into the reaction container, and slowly adding sodium hydroxide in succession to obtain liquid D;

[0179] S105, adding maleic acid and 360 parts of water into a reaction container, and dripping the D solution prepared in the step S104, and performing the first dripping of D solution. With the dripping of D solution, the temperature of the reaction system rises. When the temperature rises to 60-65°C, stop dripping D solution, add a reducing agent and hydrogen peroxide and keep the temperature for reaction for 20 minutes. After the reaction is completed, remove the heat source and drip A solution and C solution at the same time. The total dripping time of A solution is 120 minutes, and 65% is dripped in the first 60 minutes; the temperature of A solution is controlled within the range of 50-70°C during the dripping process; the total dripping time of B solution is 60 minutes, and the dripping starts 30 minutes after the A solution is dripped, and the dripping is carried out at a uniform speed throughout the whole process; the total dripping time of C solution is 60 minutes, and the C solution is dripped at a uniform speed throughout the whole process. After the dripping of A solution, B solution and C solution is completed, the second dripping of D solution is started, and the dripping speed of D solution is continuously adjusted during the period to keep the temperature in the reaction container not higher than 70°C. After all the reactions are completed, the dispersant is obtained.

[0180] S20, adding water to 12 parts of thickener, 12 parts of preservative and 20 parts of the dispersant obtained in step S105, and making the volume to 500 mL, to obtain the anti-segregation agent.

[0181] Comparative Example 3

[0182] The anti-segregation agent of Comparative Example 3 includes a dispersant, a thickener and a preservative;

[0183] Among them, the type, ratio and preparation method of the raw materials of the dispersant are the same as those in Example 7.

[0184] In the anti-segregation agent of Comparative Example 3, the thickener comprises the following raw materials in parts by weight:

[0185] The thickener comprises: 50 parts of sodium carboxymethyl cellulose, 40 parts of agar, 8 parts of xanthan gum and 7 parts of wenlun gum.

[0186] The preservatives include: 5 parts of isothiazolinone, 3 parts of 2-benzisothiazolin-3-one, 3 parts of fatty alcohol polyoxyethylene ether AEO-3, and 10 parts of 3 parts of water.

[0187] The preparation method of the anti-segregation agent in Comparative Example 3 comprises the following steps:

[0188] S10, using the dispersant prepared in Example 7 as the dispersant in this comparative example;

[0189] S201, adding sodium carboxymethyl cellulose, agar, xanthan gum and vinblastine gum into a reaction container, stirring and mixing to prepare a thickener;

[0190] S202, adding isothiazolinone, 2-benzisothiazolin-3-one, fatty alcohol polyoxyethylene ether AEO-3 and water into a reaction container, stirring and mixing to prepare a preservative;

[0191] S203, adding water to 12 parts of the thickener prepared in step S201, 20 parts of the dispersant prepared in step S105 and 12 parts of the preservative prepared in step S202 to make the volume to 500 mL, to prepare the anti-segregation agent.

[0192] Performance test 1:

[0193] The anti-segregation agents prepared in Examples 1 to 10 and Comparative Examples 1 to 3 were subjected to the following experiments:

[0194] 50g of cement and 450g of water were added to a 500ml glass beaker, and 0.5g of the anti-segregation agent prepared in Examples 1 to 10 and Comparative Example 1 was added respectively to prepare a cement slurry with a mass fraction of 10%. The performance test results are shown in Table 3.

[0195] Table 3

[0196] Time required for cement slurry to settle completely (min) Post-settlement phenomenon Example 1 ＞100 Not completely transparent, no suspended particles Example 2 ＞100 Not completely transparent, no suspended particles Example 3 ＞100 Not completely transparent, no suspended particles Example 4 ＞100 Not completely transparent, no suspended particles Example 5 ＞100 Not completely transparent, no suspended particles Example 6 ＞120 Not completely transparent, fine particles can still be suspended in the liquid Example 7 ＞120 Not completely transparent, fine particles can still be suspended in the liquid Example 8 ＞120 Not completely transparent, fine particles can still be suspended in the liquid Example 9 ＞120 Not completely transparent, fine particles can still be suspended in the liquid Example 10 ＞120 Not completely transparent, fine particles can still be suspended in the liquid Comparative Example 1 ＜60 Completely transparent, with flocculent material at the bottom Comparative Example 2 ＜30 Completely transparent, with flocculent material at the bottom Comparative Example 3 ＜30 Completely transparent, with flocculent material at the bottom

[0197] By analyzing the data in Table 3, it can be obtained that the effects of the anti-segregation agents in Examples 1 to 10 are significantly better than those in Comparative Examples 1 to 3, and the effects of the anti-segregation agents in Examples 6 to 10 are significantly better than those in Examples 1 to 5. It can be seen that the dispersant in the anti-segregation agent of the present invention selects monomers with specific functional groups to be grafted onto the main chain through copolymerization, so that the prepared anti-segregation agent has strong dispersibility and greatly improves the segregation phenomenon of the concrete mixture; at the same time, the dispersant in the anti-segregation agent of the present invention interacts with the thickener and preservative of specific components to further enhance the dispersibility of the anti-segregation agent.

[0198] Performance Test 2:

[0199] C40 concrete material was prepared with reference to the mix ratio in Table 4, and a blank group and a control group were set up respectively, wherein the blank group adopted the original mix ratio of C40 concrete material; the control group added 0.5wt% of the anti-segregation agent in Example 7 on the basis of the original mix ratio of C40 concrete material; the blank group and the control group were subjected to slump, expansion, expansion time test, gap passability J-ring expansion, inverted slump cone outflow time, stickiness, sand content, cohesion, water retention, workability, apparent density, concrete mixture anti-segregation performance, 28d compressive strength test and other performance tests, and the measurement results are shown in Table 5.

[0200] Table 4

[0201]

[0202]

[0203] Among them, the specific sources of C40 concrete are as follows:

[0204] Cement: China Resources Cement Fengkai Co., Ltd.;

[0205] Artificial sand: Huizhou Jiaotong Shenshan Green Modern Stone Quarry Co., Ltd.;

[0206] 5-10 Crushed stone: Huizhou Jiaotong Shenshan Green Modern Stone Quarry Co., Ltd.

[0207] 10-20 Crushed stone: Huizhou Jiaotong Shenshan Green Modern Stone Quarry Co., Ltd.;

[0208] Admixture: Guangdong Redwall New Materials Co., Ltd.

[0209] Fly ash: Shenzhen Energy Hehe Electric Power (Heyuan) Co., Ltd.

[0210] Table 5

[0211]

[0212] The above description is only an exemplary embodiment of the present invention, and does not limit the patent scope of the present invention. All equivalent structural changes made by using the contents of the present invention specification under the technical concept of the present invention, or direct / indirect application in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. An anti-segregation agent, characterized in that: The anti-segregation agent includes a dispersant, a thickener and a preservative; The dispersant includes a copolymer obtained from a reaction monomer under the action of an initiator; The reactive monomers include an unsaturated carboxylic acid monomer and a first monomer; Wherein, the first monomer includes at least one of a sulfonic acid monomer, an organic silicon monomer, an aromatic monomer and a phosphate ester monomer.

2. The anti-segregation agent according to claim 1, characterized in that The reactive monomers include unsaturated carboxylic acid monomers and sulfonic acid monomers, silicone monomers, aromatic monomers, and phosphate monomers. The weight ratio of the unsaturated carboxylic acid monomer, the sulfonic acid monomer, the silicone monomer, the aromatic monomer and the phosphate monomer is (200-380): (0.5-1): (10-18): (20-30): (2-5).

3. The anti-segregation agent according to claim 1, characterized in that In the reaction monomers, The unsaturated carboxylic acid monomer includes at least one of itaconic acid, methacrylic acid, maleic acid, maleic anhydride, fumaric acid, aconitic acid, fumaric acid, methyl fumaric acid, acrylic acid, angelic acid, crotonic acid, isocrotonic acid butenoic acid, and propylene tricarboxylic acid; And / or, the sulfonic acid monomer includes at least one of sodium styrene sulfonate, sodium p-styrene sulfonate, sodium methacrylic acid sulfonate, sodium vinyl sulfonate, 2-acrylamido-2-methylpropane sulfonic acid, 2-sulfoethyl methacrylate, sulfopropyl acrylate, and sulfopropyl methacrylate; And / or, the organosilicon monomer includes at least one of vinyl tri(β-methoxyethoxy)silane, vinyl triethoxysilane, vinyl trimethoxysilane, vinyl triisopropoxysiloxane, and vinyl tri(2-methoxyethoxy)silane; And / or, the aromatic monomer includes at least one of 2-phenoxyethyl acrylate and diethylene glycol phthalate diacrylate; And / or, the phosphate monomer includes at least one of methacrylate phosphate and 2-hydroxyethyl methacrylate phosphate.

4. The anti-segregation agent according to claim 1, characterized in that The reactive monomer further comprises a second monomer, wherein the second monomer is a functional monomer. Wherein, the functional monomer includes at least one of methoxy polyethylene glycol (meth) acrylate, poly (ethylene glycol) methacrylate, tetradecyl acrylate, hexadecyl acrylate, and poly (ethylene glycol) methyl ether methacrylate; and / or, in the reaction monomers, the weight ratio of the unsaturated carboxylic acid monomer, sulfonic acid monomer, silicone monomer, aromatic monomer, phosphate monomer and functional monomer is (200-380): (0.5-1): (10-18): (20-30): (2-5): (40-50).

5. The anti-segregation agent according to claim 1, characterized in that The dispersant comprises the following raw materials in parts by weight: Reaction monomer: 232.5-484 parts; Initiator: 6-8 parts; Hydrogen peroxide: 0.3-0.6 parts; Sodium hydroxide: 180-220 parts; Reducing agent: 12-27 parts; Water: 770-980 parts.

6. The anti-segregation agent according to claim 1, characterized in that In the anti-segregation agent, the weight ratio of the dispersant, the thickener and the preservative is 20:(10-13):(10-12).

7. The anti-segregation agent according to claim 1, characterized in that In the anti-segregation agent, The thickener includes at least one of guar gum, xanthan gum, wenlun gum, tapioca gum, potato gum, carrageenan, dextrin and titanium dioxide; And / or, the preservative includes at least one of isothiazolinone, 2-benzisothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, isoflavones, myricetin, 5,7-dihydroxyflavone, and soybean flavonoids.

8. A method for preparing the anti-segregation agent according to any one of claims 1 to 7, characterized in that: The preparation method of the anti-segregation agent comprises the following steps: S10, adding a reaction monomer into a reaction container, adding an initiator, reacting, and obtaining a dispersant; S20, adding a thickener and a preservative into another reaction container and mixing, adding the dispersant prepared in step S10, stirring and mixing, and preparing the anti-segregation agent.

9. The method for preparing the anti-segregation agent according to claim 8, characterized in that: The preparation method of the anti-segregation agent comprises the following steps: S101, add 90-130 parts of water and 6-8 parts of initiator to a reaction container, stir to dissolve, add 0.5-1 parts of sulfonic acid monomer and 120-150 parts of unsaturated carboxylic acid monomer, stir to mix, add 10-18 parts of organosilicon monomer, stir to mix, and prepare liquid A; S102, adding 50-60 parts of water, 2-5 parts of phosphate monomers and 20-30 parts of aromatic monomers into a reaction container, stirring and mixing, to obtain liquid B; S103, adding 50-60 parts of water and 40-50 parts of functional monomers into a reaction container, stirring and mixing, to obtain liquid C; S104, adding 280-330 parts of water into a reaction container, and gradually and slowly adding a total amount of 180-220 parts of sodium hydroxide to obtain a D solution; S105, adding 350-400 parts of water and 200-230 parts of unsaturated carboxylic acid monomers into a reaction container, stirring to dissolve, and dripping the D solution prepared in step S104, performing the first dripping of D solution, with the dripping of D solution, the temperature of the reaction system rises, when the temperature rises to 60-65° C., stopping the dripping of D solution, adding 12-27 parts of a reducing agent and 0.3-0.6 parts of hydrogen peroxide and keeping the temperature for reaction for 20 minutes, after the reaction is completed, removing the heat source and dripping A solution, 30 minutes after the dripping of A solution, starting to drip B solution, 70 minutes after the dripping of A solution, starting to drip C solution, 20 minutes after the dripping of C solution, adding the remaining D solution, performing the second dripping of D solution, after all reactions are completed, the dispersant is obtained; S201, adding 50-60 parts of hydroxypropyl guar gum with an average viscosity of 1500, 30-40 parts of hydroxypropyl guar gum with an average viscosity of 4000, 6-10 parts of xanthan gum and 5-8 parts of vinblastine gum into a reaction container, stirring and mixing to prepare a thickener; S202, adding 3 to 6 parts of isothiazolinone, 1 to 3 parts of 2-benzisothiazolin-3-one, 3 to 5 parts of 2-methyl-4-isothiazolin-3-one, 8 to 10 parts of isoflavones and 5 to 10 parts of water into a reaction container, stirring and mixing to obtain a preservative; S203, adding 10 to 13 parts of the thickener prepared in step S201, 20 parts of the dispersant prepared in step S105 and 10 to 12 parts of the preservative prepared in step S202, and making the volume to 500 mL to prepare the anti-segregation agent; In the step S105, when the D solution is dripped for the first time, the dripping rate is controlled to be 120 portions per hour; In the step S105, when the liquid A is dripped, the total dripping time is controlled to be 120 minutes, and 65% of the total amount of the liquid A is dripped in the first half of the total dripping time, and the temperature of the reaction system is controlled at 50-70° C. during the dripping process; In the step S105, when the B solution is added dropwise, the total addition time of the B solution is controlled to be 60 minutes; In the step S105, when the C solution is added dropwise, the total addition time of the C solution is controlled to be 60 minutes; In the step S105, when the D solution is dripped for the second time, the temperature of the reaction system is controlled at 70-85°C during the dripping process, and the total time of the first and second dripping of the D solution does not exceed 150 minutes.

10. Use of the anti-segregation agent according to claims 1 to 7 in concrete slurry.

Images