CN115477495B - Plastering mortar plasticizer and preparation method thereof - Google Patents
Plastering mortar plasticizer and preparation method thereof Download PDFInfo
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- CN115477495B CN115477495B CN202210941098.5A CN202210941098A CN115477495B CN 115477495 B CN115477495 B CN 115477495B CN 202210941098 A CN202210941098 A CN 202210941098A CN 115477495 B CN115477495 B CN 115477495B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention discloses a plastering mortar plasticizer and a preparation method thereof, wherein the plastering mortar plasticizer comprises the following raw materials: 8-10 parts of VAE emulsion, 8-10 parts of lignin, 2-3 parts of cellulose, 1-3 parts of carboxyl styrene-butadiene emulsion, 1-2 parts of surfactant, 2-3 parts of defoamer, 2-3 parts of rosin, 0.1-0.3 part of polyoxyethylene fatty alcohol ether and 0.2-0.6 part of maleic anhydride, the VAE emulsion and the carboxyl styrene-butadiene emulsion are compounded and then react with maleic anhydride, hydrophilic groups on the surface of the VAE emulsion are changed, so that the VAE emulsion and the modified rosin are compounded conveniently, the stability of a particle system formed by granulating is good, hydration reaction can be carried out simultaneously, the incoordination between the VAE emulsion material and the carboxyl styrene-butadiene emulsion material in the inside and mortar is increased under the action of the rosin, the overall stability of the mortar is increased after being mixed, the hydration speed of the mortar and the second treated material is slowed down by adding the Arabic hydrosol, gelatin and the phospholipid for one time, the homogenization of the mortar and the second treated material is guaranteed, the plasticizer is suitable for industrial use, and the preparation is convenient.
Description
Technical Field
The invention relates to a plastering mortar plasticizer, and in particular relates to a preparation method of the plastering mortar plasticizer.
Background
Plastering engineering is an important link in construction. When the construction of the building is completed, in order to protect the main body component and the final surface decoration leveling treatment, preliminary plastering decoration is carried out, and the quality of the plastering layer directly influences the protection capability of the main body component and the quality of the outermost decorative layer. If the plastering layer has quality accidents such as cracking and falling off, the main body component is damaged due to invasion of harmful media, and the hollowness and falling off of the plastering layer can lead to falling off of the surface coating layer and the facing bricks, so that the quality of the plastering layer is important.
The plastering mortar is prepared by refining high molecular polymer, organic additive, cement, cracking resistant component and auxiliary agent. The mortar is suitable for plastering the wall bodies such as aerated concrete blocks, light brickwork, shear walls and the like with high requirements on flatness and perpendicularity, and the traditional mortar is generally stirred on site, has poor construction and polarity, short service time, low binding power, large shrinkage and poor durability.
The plasticizer has the main functions of weakening the secondary valence bonds between polymers, so that the mobility of polymer molecular chains is increased, the crystallinity of polymer molecules is reduced, namely, the plasticity of the polymers is increased, and the easy harmony of mortar can be improved and the mortar performance is improved by doping the plasticizer into plastering mortar.
The addition of plasticizer can greatly increase the consistency, layering degree, water retention rate and the like of mortar, such as adding VAE emulsion to improve the breaking strength and the adhesive strength of the mortar, and adding lignin to improve the easy-to-mix property and the water retention property of the mortar, but the selection of the mortar plasticizer in the market is single, such as the use of the VAE emulsion needs manual blending, and the plasticizer has little improvement on the strength of the mortar.
Disclosure of Invention
The invention aims to solve the problem that the flexural strength, the adhesive strength, the water retention and the crack resistance of the traditional formula cannot be enhanced at the same time, and is suitable for industrial plasticizers and convenient to compound.
The second purpose of the invention is to provide a preparation method of lignin, which takes the formula and the preparation method in the first purpose as the basis, and solves the problems of overhigh porosity and reduced compressive strength of plastering mortar caused by using the formula and the method.
The third object of the present invention is to provide a preparation method of cellulose, which is based on the formulation and the preparation method in the first object, and solves the problem of early strength weakening of mortar caused by using the formulation and the preparation method.
The present invention achieves the above object by the following technical solutions,
the plastering mortar plasticizer comprises the following raw materials in parts by weight: 8-10 parts of VAE emulsion, 8-10 parts of lignin, 2-3 parts of cellulose, 1-3 parts of carboxyl butylbenzene emulsion, 1-2 parts of surfactant, 2-3 parts of defoamer, 2-3 parts of rosin, 0.1-0.3 part of polyoxyethylene fatty alcohol ether and 0.2-0.6 part of maleic anhydride.
The invention also provides a preparation method of the plasticizer, S1, rosin and liquid paraffin are mixed according to the weight ratio of (0.5-1): 1, grinding for 10-15min, adding half of maleic anhydride, stirring for reaction for 10-20min under heat preservation, adding polyoxyethylene fatty alcohol ether, heating to 90-100 ℃, and stirring for reaction for 15-20min at 25r/min to obtain mixed emulsion A;
s2, uniformly mixing the VAE emulsion and the carboxyl butylbenzene emulsion at 80-90 ℃, adding the other half of maleic anhydride, heating to 120-130 ℃, stirring at 25r/min for reaction for 30-40min, and cooling to 80-85 ℃ to obtain mixed emulsion B;
s3, cooling the mixed emulsion A to 80-85 ℃, adding the mixed emulsion B and the defoamer, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s4, uniformly mixing the first treatment substance with 5% of an aqueous solution of the Arabic sol, adding 5% of an aqueous solution of gelatin and phospholipid, mixing into a tissue triturator, emulsifying for 10-20s, dispersing at a high speed of 10000-14000r/min at a pH value of 3-4 and a temperature of 50-60 ℃ for 10-30min, cooling to a temperature below 30 ℃ for continuous, simultaneously adjusting a pH value to 7, continuously dispersing at a high speed for 10-20min, washing with deionized water until the microcapsule is settled, and freeze-drying to obtain a second treatment substance;
the weight ratio of the first treated matter, the Arabic sol aqueous solution, the gelatin aqueous solution and the phospholipid is 10:1:1: (0.2-0.5);
s5, blending the second treated matter with the residual raw materials to obtain the plasticizer.
Preferably, the method further comprises the post-treatment of the second treatment object, and specifically comprises the following steps:
dissolving sodium alginate in 50-60deg.C water solution, mixing with 10% of sorbitan fatty acid ester to obtain sodium alginate solution;
mixing the second treated matter with the anti-caking agent in the ratio of 1 (0.1-0.2), dispersing at 1000-2000r/min, spraying sodium alginate mixed solution with the mass of 5-6%, and drying to obtain the product.
Preferably, the anti-caking agent is one or a combination of more of bentonite, porous ceramic powder, starch, talcum powder and graphite powder.
The invention also provides a preparation method of lignin, which comprises the following steps:
D1. dissolving lignin by using 0.5-1.5 mol/L sodium hydroxide solution, regulating the pH of the solution to 10-12, heating in water bath to 40-50 ℃, adding phenol, reacting 2-4 h, cooling, and regulating the pH of the solution to 6 by using 10-15% hydrochloric acid by mass fraction to obtain a first reactant;
D2. heating the first reactant to 60-90 ℃ in water bath, adding half of chloroacetic acid, carrying out heat preservation reaction for 1-2h, adding the other half of chloroacetic acid, carrying out heat preservation reaction for 1-2h, naturally cooling, regulating pH to 7, centrifuging, removing impurities from the precipitate, and drying the obtained product below 5 ℃ to obtain lignin;
the addition amount of the chloroacetic acid is 20-50% of the mass of the lignin.
The invention also provides a preparation method of the cellulose, which comprises the following steps: the method comprises the following steps:
dissolving sodium alginate in deionized water to obtain solution A, wherein the mass of sodium alginate is kept to be 5-10%;
adding cellulose at 60-90deg.C, maintaining cellulose mass at 5-6% concentration, stirring to dissolve completely, adding into solution A system, and mixing to obtain solution B;
adding 0.01-0.1 part by mass of chelating agent into the solution B, dropwise adding the solution B added with the chelating agent into the solution B under the stirring state of 2500r/min of 10% calcium salt solution, keeping the rotating speed for reacting for 2-3 hours, cooling to below 5 ℃, standing for 5-12 hours, carrying out suction filtration, and washing to be neutral by deionized water below 5 ℃ to obtain a cellulose precursor;
weight ratio 1: mixing hydrochloric acid aqueous solution with the mass fraction of 20% with cellulose precursor (0.2-0.5), adding sodium periodate with the molar quantity of 10-50% of the cellulose precursor, regulating the pH value to 6-7, stirring and reacting at 30-40 ℃ in a dark place for 12-15h, adding ethanol with the precipitation amount for standing and precipitating, and carrying out suction filtration to obtain the cellulose.
The invention has the beneficial effects that:
(1) The VAE emulsion, the carboxyl styrene-butadiene emulsion, the lignin and the methyl cellulose ether are compounded, so that the flexural strength and the adhesive strength of the mortar are improved, the easy mixing property and the water retention property of the mortar are improved, the crack resistance of the mortar is improved, and the consistency of the mortar is increased, but the quality is reduced due to the emulsion characteristics of the VAE emulsion and the carboxyl styrene-butadiene emulsion, and the lignin and the methyl cellulose ether are extremely easy to absorb water and wet, so that the plasticizer provided by the invention can be superior as an added plastering mortar system, but is not suitable for prior compounding, and is inconvenient to use.
(2) According to the invention, rosin is added into a system of a VAE emulsion and is only used as a thickening agent for thickening in the VAE emulsion system, so that rosin, maleic anhydride and polyoxyethylene fatty alcohol ether are firstly compounded, and after grafting and emulsification are improved, strong hydration reaction is carried out on the rosin, the mortar is increased, so that the mortar strength is reduced, and therefore, the improved rosin is firstly compounded with the VAE emulsion, carboxyl styrene-butadiene emulsion and a defoaming agent to weaken the hydration property of the rosin, but hydrophilic groups of hydroxyl are generated on the surface of the VAE emulsion when the VAE emulsion is dissolved, and a separation state is generated when the modified rosin is compounded, and the viscosity of the rosin is relatively high, and after mixing with VAE particles, the viscosity of the system is reduced, so that the VAE emulsion and the carboxyl styrene-butadiene emulsion react with maleic anhydride, the surface groups of the VAE emulsion are changed, the modified rosin is conveniently compounded, the stability of a particle system formed by granulating is good, and the hydration reaction can be carried out simultaneously, so that the liability of the adhesive properties of the VAE emulsion material and the carboxyl styrene-butadiene emulsion material in the inside and the mortar under the action of the rosin is increased, and the mortar is stable, and the adhesive strength of the adhesive is increased after mixing with the mortar is increased.
(3) The second treated matter is subjected to primary microencapsulation by adding the Arabic hydrosol, the gelatin and the phospholipid, so that the hydration speed of the mortar and the second treated matter is slowed down, the homogenization in the system is carried out, the stability in the system is ensured, and meanwhile, the plasticizer is suitable for industrial use and is convenient to prepare.
(4) The existence of hydroxyl groups in lignin molecules to Ca 2+ The invention relates to a modified lignin, which is characterized in that when a large amount of hydroxyl groups exist in molecules, the complex can inhibit the crystal form development of hydration products in mortar, the crystal form development is not completely structurally changed to be fine, the air entraining effect of lignin can increase the pore volume in the mortar, the compressive strength of the mortar is not improved or even is particularly reduced, and the modified lignin is modified to reduce the hydroxyl groups in lignin functional groups and reduce Ca 2+ To improve the comprehensive strength of the mortar.
(5) The modified rosin is compounded with the VAE emulsion and the carboxyl styrene-butadiene emulsion to cause hydration reaction with the mortar in the system, although the mixing degree of the VAE emulsion and the carboxyl styrene-butadiene emulsion with the mortar can be improved, the mixed product is mixed in the mortar and is used together with the treated lignin, the later strength of the mortar can be obviously improved, but the early strength of the mortar is seriously weakened, so that the mortar cracks when in use, the problem is solved poorly by coating the primary core-shell structure, the early strength of the mortar is obviously weakened, and therefore, the sodium alginate is sprayed outside the core-shell structure to obtain a double-layer core-shell structure, the hydration of the mixed emulsion and the rosin modified is improved, the slow release effect is better, the hydration reaction of the second treated product and the mortar is slowed down and prolonged, the VAE emulsion and the carboxyl styrene-butadiene emulsion thicken the mortar at the same time of the hydration reaction, and the chemical property in the system is increased, and the early strength of the mortar is improved.
(6) The invention carries out covalent bonding and crosslinking reaction on cellulose/sodium alginate, converts hydroxyl on the surface of cellulose into carboxyl and is compounded with sodium alginate, thereby having stronger Ca 2+ The combination capacity, the modified lignin molecules and the components in the second treated matter are used together, so that the glass crystal structure of mineral powder can be destroyed, and the mineral powder can be subjected to gel recombination, thereby remarkably improving the early strength of mortar, and the system is stable and does not generate rapid hardening.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a plastering mortar plasticizer and a preparation method thereof, wherein the plastering mortar plasticizer comprises the following components in parts by weight:
preparing lignin:
D1. dissolving lignin by using 0.1 mol/L sodium hydroxide solution, regulating the pH of the solution to 10, heating in water bath to 50 ℃, adding phenol, reacting for 3h, cooling, and regulating the pH of the solution to 6 by using 15% hydrochloric acid by mass fraction to obtain a first reactant;
D2. heating the first reactant to 90 ℃ in water bath, adding half of chloroacetic acid, carrying out heat preservation reaction for 2 hours, adding the other half of chloroacetic acid, carrying out heat preservation reaction for 1 hour, naturally cooling, adjusting the pH to 7, centrifuging, removing impurities from the precipitate, and freeze-drying the obtained product at-5 ℃ to obtain lignin;
the addition amount of chloroacetic acid is 20% of the mass of lignin.
Cellulose preparation:
dissolving sodium alginate in deionized water to obtain solution A, wherein the mass of sodium alginate is kept to be 5 percent;
adding cellulose at 80 ℃, keeping the mass of the cellulose at 5%, stirring until the cellulose is completely dissolved, adding the cellulose into a solution A system, and mixing to obtain a solution B;
adding sodium citrate with the mass fraction of 0.05% of sodium alginate into the solution B, dripping the solution B added with the chelating agent into the solution B under the stirring state at the rotating speed of 2500r/min of a 10% calcium chloride aqueous solution, keeping the rotating speed for 2.5 hours, cooling to below 5 ℃, standing for 10 hours, carrying out suction filtration, and washing to be neutral by deionized water with the temperature of minus 5 ℃ to obtain a cellulose precursor;
weight ratio 1: and 0.4, mixing a hydrochloric acid aqueous solution with the mass fraction of 20% with a cellulose precursor, adding sodium periodate with the molar quantity of 10-50% of the cellulose precursor, adjusting the pH to 7, stirring and reacting at 35 ℃ in a dark place for 13 hours, adding ethanol with the precipitation quantity for standing and precipitating, and carrying out suction filtration to obtain the cellulose.
Preparing a plastering mortar plasticizer:
s1, rosin and liquid paraffin in a weight ratio of 0.5:1, adding a half amount of maleic anhydride, carrying out heat preservation and stirring reaction for 15min, adding polyoxyethylene fatty alcohol ether, heating to 90 ℃, and carrying out stirring reaction for 20min at a rotating speed of 25r/min to obtain a mixed emulsion A;
s2, uniformly mixing the VAE emulsion and the carboxyl styrene-butadiene emulsion at 90 ℃, adding the other half of maleic anhydride, heating to 120 ℃, stirring at a rotating speed of 25r/min for reaction for 30min, and cooling to 85 ℃ to obtain a mixed emulsion B;
s3, cooling the mixed emulsion A to 85 ℃, adding the mixed emulsion B and the defoamer, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s4, uniformly mixing the first treated substance with 5% of an aqueous solution of the Arabic sol, adding 5% of an aqueous solution of gelatin and phospholipid, mixing into a tissue triturator, emulsifying for 10s, dispersing at a high speed of 12000r/min at a temperature of 55 ℃ and a pH value of 4, cooling to 20 ℃ for continuous dispersion, regulating pH value to 7, continuously dispersing at a high speed for 10min, settling microcapsules, washing to neutrality by deionized water, and freeze-drying to obtain a second treated substance;
the weight ratio of the first treated matter, the Arabic sol aqueous solution, the gelatin aqueous solution and the phospholipid is 10:1:1:0.4;
dissolving sodium alginate in 60 ℃ water solution, and mixing with sorbitan fatty acid ester with the mass of 10% of that of the sodium alginate to obtain sodium alginate solution;
mixing the second treated matter with an anti-caking agent (80% of starch and 20% of graphite powder in percentage by weight) at a ratio of 1:0.15 for 2000r/min dispersion, spraying a sodium alginate mixed solution with a mass of 5%, and drying to obtain the product;
s5, blending the third treated matter with the residual raw materials to obtain the plasticizer.
Comparative example 1
This comparative example differs from example 1 in that chloroacetic acid was replaced with potassium permanganate in the preparation of lignin.
Comparative example 2
This comparative example differs from example 1 in that lignin was not modified and was commercially available lignin.
Comparative example 3
This comparative example differs from example 1 in that the cellulose was not pretreated and was commercially available.
Comparative example 4
This comparative example differs from example 1 in that sodium alginate was replaced with gelatin when cellulose was prepared.
Comparative example 5
This comparative example differs from example 1 in that sodium citrate was replaced with sodium tartrate in the preparation of cellulose.
Comparative example 6
This comparative example differs from example 1 in that sodium periodate was replaced with osmium tetroxide (commercially available) in the preparation of cellulose.
Comparative example 7
This comparative example differs from example 1 in that the plastering mortar plasticizer is prepared:
s1, melting rosin, adding a half amount of maleic anhydride, carrying out heat preservation and stirring reaction for 15min, adding polyoxyethylene fatty alcohol ether, heating to 90 ℃, and carrying out stirring reaction for 20min at a rotating speed of 25r/min to obtain a mixed emulsion A;
s2, uniformly mixing the VAE emulsion and the carboxyl styrene-butadiene emulsion at 90 ℃, adding the other half of maleic anhydride, heating to 120 ℃, stirring at a rotating speed of 25r/min for reaction for 30min, and cooling to 85 ℃ to obtain a mixed emulsion B;
s3, cooling the mixed emulsion A to 85 ℃, adding the mixed emulsion B and the defoamer, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s4, uniformly mixing the first treated substance with 5% of an aqueous solution of the Arabic sol, adding 5% of an aqueous solution of gelatin and phospholipid, mixing into a tissue triturator, emulsifying for 10s, dispersing at a high speed of 12000r/min at a temperature of 55 ℃ and a pH value of 4, cooling to 20 ℃ for continuous dispersion, regulating pH value to 7, continuously dispersing at a high speed for 10min, settling microcapsules, washing to neutrality by deionized water, and freeze-drying to obtain a second treated substance;
the weight ratio of the first treated matter, the Arabic sol aqueous solution, the gelatin aqueous solution and the phospholipid is 10:1:1:0.4;
dissolving sodium alginate in 60 ℃ water solution, and mixing with sorbitan fatty acid ester with the mass of 10% of that of the sodium alginate to obtain sodium alginate solution;
mixing the second treated matter with an anti-caking agent (80% of starch and 20% of graphite powder in percentage by weight) at a ratio of 1:0.15 for 2000r/min dispersion, spraying a sodium alginate mixed solution with a mass of 5%, and drying to obtain the product;
s5, blending the third treated matter with the residual raw materials to obtain the plasticizer.
Comparative example 8
This comparative example differs from example 1 in that in the preparation of the plastering mortar plasticizer, the liquid paraffin in step S1 is replaced with glycerin.
Comparative example 9
This comparative example differs from example 1 in that the plastering mortar plasticizer is prepared:
s1, rosin and liquid paraffin in a weight ratio of 0.5:1, grinding for 10min, adding polyoxyethylene fatty alcohol ether, heating to 90 ℃, and stirring at 25r/min for reacting for 20min to obtain mixed emulsion A;
s2, uniformly mixing the VAE emulsion and the carboxyl butylbenzene emulsion at 90 ℃, adding maleic anhydride, heating to 120 ℃, stirring at a rotating speed of 25r/min for reaction for 30min, and cooling to 85 ℃ to obtain a mixed emulsion B;
s3, cooling the mixed emulsion A to 85 ℃, adding the mixed emulsion B and the defoamer, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s4, uniformly mixing the first treated substance with 5% of an aqueous solution of the Arabic sol, adding 5% of an aqueous solution of gelatin and phospholipid, mixing into a tissue triturator, emulsifying for 10s, dispersing at a high speed of 12000r/min at a temperature of 55 ℃ and a pH value of 4, cooling to 20 ℃ for continuous dispersion, regulating pH value to 7, continuously dispersing at a high speed for 10min, settling microcapsules, washing to neutrality by deionized water, and freeze-drying to obtain a second treated substance;
the weight ratio of the first treated matter, the Arabic sol aqueous solution, the gelatin aqueous solution and the phospholipid is 10:1:1:0.4;
dissolving sodium alginate in 60 ℃ water solution, and mixing with sorbitan fatty acid ester with the mass of 10% of that of the sodium alginate to obtain sodium alginate solution;
mixing the second treated matter with an anti-caking agent (80% of starch and 20% of graphite powder in percentage by weight) at a ratio of 1:0.15 for 2000r/min dispersion, spraying a sodium alginate mixed solution with a mass of 5%, and drying to obtain the product;
s5, blending the third treated matter with the residual raw materials to obtain the plasticizer.
Comparative example 10
The comparative example differs from example 1 in that the formulation comprises the following components in parts by weight:
preparing a plastering mortar plasticizer:
s1, uniformly mixing the VAE emulsion and the carboxyl butylbenzene emulsion at 90 ℃, adding maleic anhydride, heating to 120 ℃, stirring at a rotating speed of 25r/min for reaction for 30min, and cooling to 85 ℃ to obtain a mixed emulsion;
s2, cooling the mixed emulsion to 85 ℃, adding a defoaming agent and polyoxyethylene fatty alcohol ether, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s3, uniformly mixing the first treated substance with 5% of an aqueous solution of the Arabic sol, adding 5% of an aqueous solution of gelatin and phospholipid, mixing into a tissue triturator, emulsifying for 10s, dispersing at a high speed of 12000r/min at a temperature of 55 ℃ to 4, cooling to 20 ℃ for continuous dispersion, regulating pH to 7, continuously dispersing at a high speed for 10min, settling the microcapsules, washing to neutrality with deionized water, and freeze-drying to obtain a second treated substance;
the weight ratio of the first treated matter, the Arabic sol aqueous solution, the gelatin aqueous solution and the phospholipid is 10:1:1:0.4;
dissolving sodium alginate in 60 ℃ water solution, and mixing with sorbitan fatty acid ester with the mass of 10% of that of the sodium alginate to obtain sodium alginate solution;
mixing the second treated matter with an anti-caking agent (80% of starch and 20% of graphite powder in percentage by weight) at a ratio of 1:0.15 for 2000r/min dispersion, spraying a sodium alginate mixed solution with a mass of 5%, and drying to obtain the product;
s4, blending the third treated matter with the residual raw materials to obtain the plasticizer.
Comparative example 11
This comparative example differs from example 1 in that the plastering mortar plasticizer is prepared:
s1, rosin and liquid paraffin in a weight ratio of 0.5:1, adding a half amount of maleic anhydride, carrying out heat preservation and stirring reaction for 15min, adding polyoxyethylene fatty alcohol ether, heating to 90 ℃, and carrying out stirring reaction for 20min at a rotating speed of 25r/min to obtain a mixed emulsion A;
s2, uniformly mixing the VAE emulsion and the carboxyl styrene-butadiene emulsion at 90 ℃, adding the other half of maleic anhydride, heating to 120 ℃, stirring at a rotating speed of 25r/min for reaction for 30min, and cooling to 85 ℃ to obtain a mixed emulsion B;
s3, cooling the mixed emulsion A to 85 ℃, adding the mixed emulsion B and the defoamer, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s4, uniformly mixing the first treatment substance with 5% of cholesterol, adding 5% of phospholipid, mixing to obtain a composition, dispersing a phosphate buffer with the pH value of 7 at a high speed at 50 ℃, dropwise adding the composition while keeping a dispersion state, dispersing for 15min at a speed of 12000r/min, cooling to 20 ℃ for continuous dispersion, washing with deionized water to be neutral after the microcapsule is settled, and freeze-drying to obtain a second treatment substance;
the weight ratio of the first treated matter to the cholesterol to the phospholipid is 1:1:0.4;
dissolving sodium alginate in 60 ℃ water solution, and mixing with sorbitan fatty acid ester with the mass of 10% of that of the sodium alginate to obtain sodium alginate solution;
mixing the second treated matter with an anti-caking agent (80% of starch and 20% of graphite powder in percentage by weight) at a ratio of 1:0.15 for 2000r/min dispersion, spraying a sodium alginate mixed solution with a mass of 5%, and drying to obtain the product;
s5, blending the third treated matter with the residual raw materials to obtain the plasticizer.
Comparative example 12
This comparative example differs from example 1 in that no sorbitan fatty acid ester was added in step S4 when the plastering mortar plasticizer was prepared.
Comparative example 13
This comparative example differs from example 1 in that the plastering mortar plasticizer is prepared: s1, rosin and liquid paraffin in a weight ratio of 0.5:1, adding a half amount of maleic anhydride, carrying out heat preservation and stirring reaction for 15min, adding polyoxyethylene fatty alcohol ether, heating to 90 ℃, and carrying out stirring reaction for 20min at a rotating speed of 25r/min to obtain a mixed emulsion A;
s2, uniformly mixing the VAE emulsion and the carboxyl styrene-butadiene emulsion at 90 ℃, adding the other half of maleic anhydride, heating to 120 ℃, stirring at a rotating speed of 25r/min for reaction for 30min, and cooling to 85 ℃ to obtain a mixed emulsion B;
s3, cooling the mixed emulsion A to 85 ℃, adding the mixed emulsion B and the defoamer, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s4, uniformly mixing the first treated substance with 5% of an aqueous solution of the Arabic sol, adding 5% of an aqueous solution of gelatin and phospholipid, mixing into a tissue triturator, emulsifying for 10s, dispersing at a high speed of 12000r/min at a temperature of 55 ℃ and a pH value of 4, cooling to 20 ℃ for continuous dispersion, regulating pH value to 7, continuously dispersing at a high speed for 10min, settling microcapsules, washing to neutrality by deionized water, and freeze-drying to obtain a second treated substance;
the weight ratio of the first treated matter, the Arabic sol aqueous solution, the gelatin aqueous solution and the phospholipid is 10:1:1:0.4;
s5, blending the third treated matter with the residual raw materials to obtain the plasticizer.
Example 2
This embodiment differs from embodiment 1 in that: the anti-caking agent comprises, by weight, 80% of bentonite and 20% of graphite powder.
1. Performance detection of plasticizers prepared according to the present invention
The plastering mortar plasticizers prepared in examples 1 to 2 and comparative examples 1 to 13 of the present invention were added to a reference mortar with reference to JG/T426-2013 "plastering mortar plasticizer" standard, and the air content, the air content 1h variation, the water retention rate and the state of the mixture were tested, and the specific results are shown in table 1:
TABLE 1
The plastering mortar plasticizers prepared in examples 1 to 2 and comparative examples 1 to 13 of the present invention were added to a reference mortar and tested for flexural strength and compressive strength, and the specific results are shown in table 2:
TABLE 2
As can be seen from the results in tables 1-2, the plasticizer prepared by the formulation and the method in examples 1-2 of the present invention can significantly improve the working performance of the plastering mortar, and has the advantages of no bleeding, moderate air content, low air content change, high water retention, proper consistency, low consistency loss, high overall performance, namely, mortar stability, and no decrease in the strength of the mortar 7d, particularly improvement, so that the plasticizer in examples 1-2 of the present invention actually improves the working performance of the plastering mortar while maintaining the mechanical properties thereof, and achieves the balance of the two.
Comparing examples 1-2, it is clear that, in example 2, the mechanical properties and working properties of the anti-caking agent are reduced to a small extent due to the component adjustment, but still the anti-caking agent still accords with the national standard of JG/T426-2013 "plastering mortar plasticizer", and the mechanical properties are improved.
As is clear from comparative examples 1 and 1-2, the lignin modifying component is adjusted in comparative example 1, the working performance and mechanical properties are far lower than those of example 1, especially the mechanical properties are obviously reduced, and the lignin is not modified in comparative example 2, so that the working performance is obviously reduced.
As is clear from comparative examples 1 and 3 to 6, comparative example 3, in which the cellulose was not modified, resulted in a significant decrease in the mechanical properties of 7d, and comparative examples 4 to 6, in which the components of the cellulose were modified, showed a significant decrease in the mechanical properties.
As is clear from comparative examples 1 and comparative examples 7 to 13, comparative examples 7 to 9, in which the rosin treatment mode and the treatment composition were modified, showed a small decrease in the working properties, but showed a significant decrease in the later flexural strength, and comparative example 10, in which no rosin component was added, showed a large decrease in the flexural strength, compressive strength and working properties, and comparative examples 11 to 12, in which the core-shell structure was modified, showed no performance comparable to that of example 1.
From the above, compared with the plastering mortar plasticizers prepared in example 2 and comparative examples 1 to 13, the working performance of the plastering mortar can be improved after the plastering mortar plasticizer is added, and on the basis of moderate air content and proper consistency, the air content change degree is the lowest, the water retention rate is the highest, the consistency loss is the lowest, and the early-stage and late-stage mechanical properties are the best, so that example 1 is considered as the best example of the invention.
The above description is merely a preferred embodiment of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the concept of the invention belong to the protection scope of the invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (2)
1. The plastering mortar plasticizer is characterized by comprising the following raw materials in parts by weight: 8-10 parts of VAE emulsion, 8-10 parts of modified lignin, 2-3 parts of modified cellulose, 1-3 parts of carboxyl butylbenzene emulsion, 1-2 parts of surfactant, 2-3 parts of defoamer, 2-3 parts of rosin, 0.1-0.3 part of polyoxyethylene fatty alcohol ether and 0.2-0.6 part of maleic anhydride;
the preparation method of the plastering mortar plasticizer comprises the following steps:
s1, rosin and liquid paraffin in a weight ratio of (0.5-1): 1. grinding for 10-15min, adding half amount of maleic anhydride, stirring for reacting for 10-20min under heat preservation, adding polyoxyethylene fatty alcohol ether, heating to 90-100deg.C, and stirring for reacting for 15-20min at 25r/min to obtain mixed emulsion A;
s2, uniformly mixing the VAE emulsion and the carboxyl butylbenzene emulsion at 80-90 ℃, adding the other half of maleic anhydride, heating to 120-130 ℃, stirring at 25r/min for reaction for 30-40min, and cooling to 80-85 ℃ to obtain mixed emulsion B;
s3, cooling the mixed emulsion A to 80-85 ℃, adding the mixed emulsion B and the defoamer, uniformly mixing, and adjusting the pH value to 7 to obtain a first treated matter;
s4, uniformly mixing the first treated substance with 5% of an aqueous solution of the Arabic sol, adding 5% of an aqueous solution of gelatin and phospholipid, mixing into a tissue triturator, emulsifying for 10-20s, dispersing at a high speed of 10000-14000r/min for 10-30min at a temperature of 50-60 ℃ by adjusting the pH value to 3-4, cooling to a temperature below 30 ℃ for continuous, simultaneously adjusting the pH value to 7, dispersing at a high speed for 10-20min, washing with deionized water until the microcapsule is settled, and freeze-drying to obtain a second treated substance; the weight ratio of the first treated matter, the Arabic sol aqueous solution, the gelatin aqueous solution and the phospholipid is 10:1:1: (0.2-0.5);
s5, blending the second treated matter with the residual raw materials to obtain the plasticizer;
the preparation method of the plastering mortar plasticizer further comprises the post-treatment of the second treatment object, and specifically comprises the following steps:
dissolving sodium alginate in 50-60deg.C water solution, mixing with 10% of sorbitan fatty acid ester to obtain sodium alginate solution;
mixing the second treated matter with the anti-caking agent in the proportion of 1 (0.1-0.2), dispersing at a speed of 1000-2000r/min, spraying sodium alginate mixed solution with the mass of 5-6%, and drying;
the lignin modifying method comprises the following steps:
D1. dissolving lignin by using 0.5-1.5 mol/L sodium hydroxide solution, regulating the pH of the solution to 10-12, heating in water bath to 40-50 ℃, adding phenol, reacting 2-4 h, cooling, and regulating the pH of the solution to 6 by using 10-15% hydrochloric acid by mass fraction to obtain a first reactant;
D2. heating the first reactant to 60-90 ℃ in water bath, adding half of chloroacetic acid, carrying out heat preservation reaction for 1-2h, adding the other half of chloroacetic acid, carrying out heat preservation reaction for 1-2h, naturally cooling, regulating pH to 7, centrifuging, removing impurities from the precipitate, and drying the obtained product below 5 ℃ to obtain the modified lignin;
the addition amount of the chloroacetic acid is 20-50% of the mass of lignin;
the method for modifying cellulose in the plasticizer comprises the following steps:
dissolving sodium alginate in deionized water to obtain solution A, wherein the mass of sodium alginate is kept to be 5-10%;
adding cellulose at 60-90deg.C, maintaining cellulose mass at 5-6% concentration, stirring to dissolve completely, adding into solution A system, and mixing to obtain solution B;
adding chelating agent with mass fraction of 0.01-0.1% into solution B, dropwise adding solution B with chelating agent into 10% calcium salt solution in 2500r/min stirring state, keeping the rotation speed for 2-3h, cooling to below 5deg.C, standing for 5-12h, suction filtering, and washing with deionized water below 5deg.C to neutrality to obtain cellulose precursor;
weight ratio 1: (0.2-0.5) mixing 20% hydrochloric acid aqueous solution with cellulose precursor, adding 10-50% sodium periodate with the molar weight of the cellulose precursor, adjusting pH to 6-7, stirring in a dark place at 30-40 ℃ for reaction for 12-15h, adding ethanol with precipitation amount for standing precipitation, and carrying out suction filtration to obtain the modified cellulose.
2. The method for preparing the plastering mortar plasticizer according to claim 1, wherein the anti-caking agent is one or a combination of more of bentonite, porous ceramic powder, starch, talcum powder and graphite powder.
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