CN111533514A - Colored dry-mixed mortar and preparation method thereof - Google Patents
Colored dry-mixed mortar and preparation method thereof Download PDFInfo
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- CN111533514A CN111533514A CN202010398092.9A CN202010398092A CN111533514A CN 111533514 A CN111533514 A CN 111533514A CN 202010398092 A CN202010398092 A CN 202010398092A CN 111533514 A CN111533514 A CN 111533514A
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/2023—Resistance against alkali-aggregate reaction
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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Abstract
The invention provides color dry-mixed mortar and a preparation method thereof, and solves the technical problems that the color mortar in the prior art has poor weather resistance and is easy to cause efflorescence for dry-mixed mortar using portland cement as a cementing material. The preparation comprises the following components in parts by weight: 80-90 parts of machine-made sand; 10-15 parts of a mixture W; 1-10 parts of stone powder and 1-5 parts of pigment; 0.1 to 1 portion of redispersible latex powder; 0.2 to 1.2 portions of hydroxypropyl methyl cellulose ether; 10-15 parts of zeolite powder; the mixture W is prepared from white portland cement, a modified mixture T-C and N, O carboxymethyl chitosan; the modified mixture T-C is prepared from chitosan, isopropanol and ClCH2COOH and modified titanium dioxide. The color dry-mixed mortar prepared by the invention has good weather resistance, and can avoid the occurrence of saltpetering as much as possible.
Description
Technical Field
The invention relates to titanium dioxide, and particularly relates to color dry-mixed mortar and a preparation method thereof.
Background
The color mortar is one kind of special mortar for decorating inner and outer walls of building and can resist the damage of high temperature, low temperature and humidity and beautify the decorated building. It is widely used in industry and civil construction because of its bright and durable color.
With the increase of the pollution degree of the external environment and the change of the climate, the weather resistance of the color mortar is gradually reduced. The weather resistance is the tolerance capability of materials such as paint, building plastic, rubber products and the like to withstand the outdoor weather, such as comprehensive damage caused by illumination, cold and heat, wind and rain, bacteria and the like. The most obvious performance is that the color mortar is hydrated by ordinary portland cement with Ca (OH) under the action of rainwater2With the water leaching out, saltpetering occurs. The efflorescence phenomenon is commonly called whitening or blooming, and is a phenomenon frequently occurring on the surface of a building, and includes a mortar surface, a concrete surface, a clay brick surface, a tile surface and the like. The efflorescence is generally in the form of white powder, flocs or flakes. This occurs on many building walls, particularly where the rain fly and wall join, at roof drains, and on many plastered mortar surfaces. It is just like skin disease to human body to the building, is harmful to the outward appearance pleasing to the eye, seriously influences the building engineering impression quality, sometimes still can influence its colouring effect and basic unit and surface finishing, wainscot, whitewash the bonding quality of the layer, still can cause the cracking hollowing of the plastering mortar layer of the colored mortar. Therefore, during the construction of the color mortar, a layer of primer needs to be coated on the bottom layer in advance, and a side finish is made after the primer is finished, so that the purpose of preventing the color mortar from being efflorescent in a complex environment later is achieved.
In foreign countries, the phenomena of Efflorescence such as masonry walls have been described in large numbers in the early 19 th century, and Ritchie published the article Efflorescence in 1960. In the future, researchers have conducted a great deal of research on the problem of the ubiquitination, and have many research results on the formation mechanism and the prevention approach of the ubiquitination. Through a great deal of research by domestic and foreign scientists, it has been found that the whiskering of cement systems is caused by the fact that soluble components in materials such as cement, sand, stone and admixtures are dissolved in water and then precipitate on the surface of a hardened body or react with CO in the air along with the evaporation of water on the surface of mortar2And the like to produce a white deposit. The chemical components of the white substances are changed according to the used materials,The construction process and the time, season, environment, etc. of the construction are different. According to the X-ray diffraction analysis result, Ca (OH) is common2、CaCO3、CaSO4、Na2SO4、Na2CO3、K2CO3And the like. For dry-mixed mortars using portland cement as cementitious material, the result is Ca (OH)2Is itself a hydration product, and is almost unavoidable for efflorescence.
The applicant has found that the prior art has at least the following technical problems:
the color mortar in the prior art has poor weather resistance, and is easy to cause efflorescence for dry-mixed mortar using portland cement as a cementing material.
Disclosure of Invention
The invention aims to provide color dry-mixed mortar and a preparation method thereof, and aims to solve the technical problems that the color mortar in the prior art is poor in weather resistance and is easy to cause efflorescence for dry-mixed mortar using portland cement as a cementing material. The technical effects that can be produced by the preferred technical scheme in the technical schemes provided by the invention are described in detail in the following.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides color dry-mixed mortar, which is prepared from the following components in parts by weight:
80-90 parts of machine-made sand;
10-15 parts of a mixture W;
1 to 10 parts of stone powder,
1-5 parts of pigment;
0.1 to 1 portion of redispersible latex powder;
0.2 to 1.2 portions of hydroxypropyl methyl cellulose ether;
10-15 parts of zeolite powder;
the mixture W is prepared from white portland cement, a modified mixture T-C and N, O carboxymethyl chitosan; the weight percentage content of calcium oxide in the white portland cement is 58-65%;
the modified mixture T-C is prepared from chitosan, isopropanol and ClCH2COOH and modified titanium dioxide.
Further, the weight parts of the components are respectively as follows:
82-88 parts of machine-made sand;
12-14 parts of a mixture W;
3 to 8 portions of stone powder,
2-4 parts of pigment;
0.3 to 0.8 portion of redispersible latex powder;
0.4 to 1 part of hydroxypropyl methyl cellulose ether;
11 to 14 portions of zeolite powder.
Further, the weight parts of the components are respectively as follows:
85 parts of machine-made sand;
12 parts of a mixture W;
6 parts of stone powder, namely 6 parts of stone powder,
3 parts of a pigment;
0.5 part of redispersible latex powder;
0.8 part of hydroxypropyl methyl cellulose ether;
12 parts of zeolite powder.
Further, the preparation of the mixture W comprises the following raw materials in parts by weight:
20-25 parts of white portland cement;
10-15 parts of modified mixture T-C;
0.1 to 0.5 portion of N, O carboxymethyl chitosan.
Further, the preparation of the mixture W comprises the following raw materials in parts by weight:
22-24 parts of white portland cement;
11-14 parts of modified mixture T-C;
0.2 to 0.4 portion of N, O carboxymethyl chitosan.
Further, the modified mixture T-C is prepared from the following raw materials in parts by weight:
0.5-1.5 parts of chitosan;
8-12 parts of isopropanol;
ClCH21-2 parts of COOH;
85-90 parts of modified titanium dioxide.
Further, the modified mixture T-C is prepared from the following raw materials in parts by weight:
1 part of chitosan
10 portions of isopropanol
ClCH2COOH 1.5 parts
87 parts of modified titanium dioxide.
The preparation method of the color dry-mixed mortar provided by the invention comprises the following steps:
(1) preparation of modified titanium white powder
A1, adding butyl titanate into a reactor, and gasifying the butyl titanate at the temperature of 40-130 ℃ under the protection of inert gas;
a2, adding water into a reactor, reacting at 500-550 ℃ and 0.5 × 105Pa～1.5×105Pa, inert gas protection to obtain nano TiO2；
A3, and the nanometer TiO obtained in the step A22Placing the mixture in an inert gas atmosphere to reduce the temperature to 20-25 ℃;
a4, cooling the TiO obtained in the step A32Carrying out screen analysis to obtain a finished product of the modified titanium dioxide;
the chemical reaction process can be expressed by the following chemical reaction equation:
Ti(OC4H9)4+2H2O→TiO2+4C4H9OH
(2) preparation of modified mixture T-C
B1, adding chitosan and NaOH solution into a reaction container, and alkalizing the chitosan in the NaOH solution;
b2, adding isopropanol and ClCH into the reaction vessel in sequence2COOH is evenly stirred and then is placed for 2 to 3 hours at the temperature of between 15 and 25 ℃; then heating to 65-70 ℃, and preserving the heat for 1.5-2 h; then adjusting the pH value to 6-8;
b3, adding the modified titanium dioxide prepared in the step (1) into a reaction container, uniformly stirring to obtain a mixture, filtering the mixture, and keeping a precipitate;
b4, using CH in turn for the precipitate obtained in the step B33CH2Washing with OH solution and anhydrous methanol to ensure the activation of chitosan and maintain the activity of titanium pigment;
b5, drying at 50-70 ℃ after washing to obtain a modified mixture T-C;
(3) preparation of N, O carboxymethyl chitosan
C1, dissolving the modified mixture T-C prepared in the step (2) in water at the temperature of 30-40 ℃ to obtain a solution a;
c2, adding CH to the solution a obtained in the step C13OCH3Carrying out precipitation reaction on the solution, filtering after the reaction is finished, and keeping the precipitate;
c3 precipitation obtained in step C2 with anhydrous CH3CH2OH washing, and then vacuum drying to obtain N, O carboxymethyl chitosan powder;
(4) preparation of mixture W
Uniformly mixing white portland cement, the modified mixture T-C obtained in the step (2) and the N, O carboxymethyl chitosan obtained in the step (3) according to a ratio to obtain a mixture W;
(5) preparation of finished product of colored dry-mixed mortar
And uniformly mixing the machine-made sand, the mixture W, the stone powder, the pigment, the redispersible latex powder, the hydroxypropyl methyl cellulose ether and the zeolite powder according to the proportion to obtain a finished product of the color dry-mixed mortar.
Further, in the step (1) A4, the sieve analysis is to cool the TiO obtained in the step (1) A32Placing in a 45 μm round hole sieve, and controlling TiO2The content is more than 98%, the screen residue is less than 0.01%, the volatile matter at 105 ℃ is less than 0.05%, and the L value range is 98.5-100.
Further, in the step (1) A2, the mass ratio of the water to the butyl titanate is 2: 1-20: 1.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) according to the color dry-mixed mortar and the preparation method provided by the invention, the modified titanium dioxide is added into the color dry-mixed mortar as a weather-resistant additive, the modified titanium dioxide is in an anatase structure, the anatase structure can reflect a large amount of visible light of 400-700 nm, and simultaneously absorbs the ultraviolet light of 300-400 nm which is larger than that of rutile titanium dioxide, the temperature raising capability of the visible light is strong, so that the internal temperature of the mortar is raised, the cement paste and the polymer are separated from each other due to the fact that the thermal expansion coefficients of the cement paste and the polymer are different, and meanwhile, the polymer film is aged and cannot be compounded with the cement paste due to the fact that the polymerization is irradiated by the ultraviolet light and the cross-linked molecules; the added modified nano titanium dioxide can reflect a large amount of visible light by absorbing ultraviolet light through the modified nano titanium dioxide, so that the color vividness is enhanced; the added modified titanium dioxide can ensure that a polymer in the cement paste and the cement paste can not be separated from each other due to the difference of linear expansion coefficients, so that the adhesion of the polymer to the white Portland cement and the refinement and filling of capillary pores are ensured; under the condition of low temperature, the polymer film has small elastic modulus and large linear shrinkage, the polymer film can better play a role in bonding, and the film can be better ensured to be tightly adhered to the surface of the cement paste body, so that the polymer film and the cement paste body are stably integrated.
(2) According to the colored dry-mixed mortar and the preparation method thereof, the polymer used is a hydrophobic polymer, and specifically can be redispersible latex powder (vinyl acetate and ethylene copolymer EVA), and due to the hydrophobicity, the colored dry-mixed mortar can ensure that external moisture cannot infiltrate the mortar slurry, and the hydrophobic polymer ensures that the cement slurry is not eroded by the external moisture, and ensures the contribution of the polymer to the mortar slurry under the condition of no high temperature.
(3) The invention provides color dry-mixed mortar and a preparation method thereof, wherein pigment and zeolite powder are added in the color mortar as active admixture, and Ca (OH) is generated in cement hydration products2In the process, the excessive calcium hydroxide reacts with the active admixture, the excessive calcium hydroxide is consumed to inhibit the efflorescence of the mortar under the dry-wet cycle, and the inside of the mortar is carbonized to prevent the reduction of the alkalinity of the cement paste caused by the excessive calcium hydroxideThe polymer (redispersible latex powder, namely vinyl acetate and ethylene copolymer EVA) is attached to the surfaces of the hydration products C-S-H gel, so that the contact of carbon dioxide in the air and cement slurry can be prevented; moreover, the zeolite powder used in the invention is a white pigment, can be used as a pigment, has volcanic ash activity, can consume calcium hydroxide generated by cement hydration, and avoids the whiskering phenomenon of color mortar; in addition, the zeolite powder used is a porous admixture, can carry a large amount of water, does not consume the water in the system in the early stage, and can fully ensure the water demand of the color mortar in the later stage.
(4) According to the color dry-mixed mortar and the preparation method thereof, when the color pigment is not added, the color of the product is strong fluorescent white, and other color pigments are added on the basis of the strong fluorescent white, so that the color pigment has a good background color, a prominent setoff effect, a bright product color and incomparable advantages of other color mortars.
(5) According to the color dry-mixed mortar and the preparation method thereof, when the prepared color dry-mixed mortar is constructed, priming and plastering can be directly carried out according to the operation of the traditional plastering mortar, the construction is extremely convenient, two construction procedures (a finishing paint coating procedure and a bottom surface plastering mortar procedure) can be reduced in the construction, and the construction efficiency can be improved by 200%; in addition, only redispersible latex powder (EVA) and a small amount of PVA (the redispersible latex powder is a compound and contains PVA as a protective layer) are used for protection during preparation; the pigment is used for adjusting the color of the common sandstone, so that the preparation cost can be reduced, and the investment can be reduced.
(6) According to the color dry-mixed mortar and the preparation method thereof provided by the invention, the prepared color dry-mixed mortar has breathability, N, O carboxymethyl chitosan can release adsorbed moisture by itself under dry weather, N, O carboxymethyl chitosan has good hygroscopicity and moisture retention type under humid weather or rainy weather, a wall body can be kept in a dry state, the erosion of rainwater can be avoided in a high-humidity environment outside the wall body, and the joint water prevention of a polymer and a mortar system is realized.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
First, preparation example:
the following raw materials are illustrated in examples 1 to 5:
white portland cement: the WPC strength grade is 42.5R, and the CaO content is 58% -65%: the whiteness is more than 80 percent;
and (3) machining sand: SiO 22The content is more than 70 percent, the fineness modulus FM ranges from 1.5 to 1.8, the maximum particle size of the particles is less than 2.36mm, and the content of the particles with the particle size of less than 75 mu m is 10 to 15 percent;
stone powder: CaCO3The content is more than 90 percent, and the content of particles with the particle diameter of less than 75 mu m is 90 to 95 percent;
pigment: is one or more of iron oxide yellow, iron oxide green and iron oxide red; certainly, blending is carried out according to the color requirement;
redispersible latex powder (EVA): the material is composed of a vinyl acetate-ethylene copolymer, model 5010, ash content is less than 10%, and solid content is more than 99.8%;
hydroxypropyl methylcellulose ether (HPMC): the brookfield viscosity is 10000 Pa.s-100000 Pa.s, the ash content is less than 6%, the hydroxypropyl content is 13-19%, the ash content is 2-5%, and the PH is 6-9;
zeolite powder: is clinoptilolite with whiteness of more than 80%, activity index of more than 75%, and fineness of more than 400m2The ammonium absorption value is 100mmol/100 g-150 mmol/100 g.
Example 1:
preparing color dry-mixed mortar:
(1) preparing modified titanium dioxide:
raw materials (in parts by weight): 1 part of butyl titanate and 10 parts of water;
a1, adding butyl titanate into a reactor at 85 ℃ and N2Under protection, butyl titanate is gasified;
a2, adding water into a reactor, reacting at 525 ℃ and 1.01 × 105Pa、N2Under the protection of (1L/min of nitrogen flow, 1L/min of water vapor flow and 30min of reaction time), obtaining R818 type nano TiO2；
A3, and the nanometer TiO obtained in the step A22Placing in inert gas CO2Cooling to 23 ℃ in the atmosphere;
a4, cooling the TiO obtained in the step A32Placing in a 45 μm round hole sieve, and controlling TiO2The content is more than 98 percent, the screen residue is less than 0.01 percent, the volatile matter at 105 ℃ is less than 0.05 percent, and the L value range is 98.5-100, thus obtaining the finished product of the modified titanium dioxide;
(2) preparation of modified mixture T-C
Raw materials (in parts by weight): 0.5 part of chitosan, 8 parts of isopropanol and ClCH2COOH 2 parts and modified titanium dioxide 87 parts;
b1, adding chitosan and a NaOH solution (the mass fraction is 60%) into a reaction container, wherein the mass ratio of the chitosan to the NaOH solution is 1:13, and the chitosan is alkalized in the NaOH solution;
b2, adding isopropanol and ClCH into the reaction vessel in sequence2COOH is stirred evenly and then placed for 3 hours at the temperature of 15 ℃; then heating to 65 ℃, and preserving heat for 2 hours; then using CH3Adjusting the PH value of COOH to be 8;
b3, adding the modified titanium dioxide prepared in the step (1) into a reaction container, uniformly stirring to obtain a mixture, filtering the mixture, and keeping a precipitate;
b4, using CH in turn for the precipitate obtained in the step B33CH2Washing with OH solution (70 wt%) and anhydrous methanol;
b5, drying at 50 ℃ after washing to obtain a modified mixture T-C;
(3) preparation of N, O carboxymethyl chitosan
Raw materials (in parts by weight): modified mixtureT-C, water, CH3OCH3Solution (mass fraction is 75% -80%)
C1, dissolving the modified mixture T-C prepared in the step (2) in water at the temperature of 30 ℃ to obtain a solution a;
c2, adding CH to the solution a obtained in the step C13OCH3Carrying out precipitation reaction on the solution (the mass fraction is 80%), filtering after the reaction is finished, and keeping the precipitate;
c3 precipitation obtained in step C2 with anhydrous CH3CH2OH washing (for many times), then vacuum drying, controlling the molecular weight to 50000, and obtaining N, O carboxymethyl chitosan powder (substances with the molecular weight larger than 50000 can be returned to the step (2) to be mixed with raw material chitosan for use (namely, the mixed substances are used as chitosan), and the preparation of the modified mixture T-C is continuously carried out according to the step (2);
(4) preparation of mixture W
Raw materials (in parts by weight): 20 parts of white portland cement, 10 parts of modified mixture T-C and 0.5 part of N, O carboxymethyl chitosan;
uniformly mixing white portland cement, the modified mixture T-C obtained in the step (2) and the N, O carboxymethyl chitosan obtained in the step (3) according to the proportion, and controlling the screen residue of a 80-micron square-hole screen to be less than 1% to obtain a mixture W;
(5) preparation of finished product of colored dry-mixed mortar
Raw materials (in parts by weight): 80 parts of machine-made sand, 15 parts of mixture W, 1 part of stone powder, 5 parts of pigment (iron oxide yellow), 0.1 part of redispersible latex powder, 1.2 parts of hydroxypropyl methyl cellulose ether and 10 parts of zeolite powder;
and uniformly mixing the machine-made sand, the mixture W, the stone powder, the pigment, the redispersible latex powder, the hydroxypropyl methyl cellulose ether and the zeolite powder according to the proportion to obtain a finished product of the color dry-mixed mortar.
Example 2:
preparing color dry-mixed mortar:
(1) preparing modified titanium dioxide:
raw materials (in parts by weight): 1 part of butyl titanate and 15 parts of water;
a1, addition of butyl titanate to the reactionIn the reactor, at a temperature of 60 ℃ and N2Under protection, butyl titanate is gasified;
a2, adding water into the reactor, reacting at 510 deg.C and 1.5 × 105Pa、N2Under the protection of (1L/min of nitrogen flow, 1L/min of water vapor flow and 30min of reaction time), obtaining R818 type nano TiO2；
A3, and the nanometer TiO obtained in the step A22Placing in inert gas CO2Cooling to 22 ℃ in the atmosphere;
a4, cooling the TiO obtained in the step A32Placing in a 45 μm round hole sieve, and controlling TiO2The content is more than 98 percent, the screen residue is less than 0.01 percent, the volatile matter at 105 ℃ is less than 0.05 percent, and the L value range is 98.5-100, thus obtaining the finished product of the modified titanium dioxide;
(2) preparation of modified mixture T-C
Raw materials (in parts by weight): 1.5 parts of chitosan, 12 parts of isopropanol and ClCH21 part of COOH and 90 parts of modified titanium dioxide;
b1, adding chitosan and a NaOH solution (the mass fraction is 50%) into a reaction container, wherein the mass ratio of the chitosan to the NaOH solution is 1:15, and the chitosan is alkalized in the NaOH solution;
b2, adding isopropanol and ClCH into the reaction vessel in sequence2COOH is stirred evenly and then placed for 2 hours at the temperature of 25 ℃; then heating to 70 ℃, and preserving heat for 1.5 h; then using CH3Adjusting the PH value of COOH to be 6;
b3, adding the modified titanium dioxide prepared in the step (1) into a reaction container, uniformly stirring to obtain a mixture, filtering the mixture, and keeping a precipitate;
b4, using CH in turn for the precipitate obtained in the step B33CH2Washing with OH solution (60 wt%) and anhydrous methanol;
b5, drying at the temperature of 70 ℃ after washing to obtain a modified mixture T-C;
(3) preparation of N, O carboxymethyl chitosan
Raw materials (in parts by weight): modified mixture T-C, water, CH3OCH3Solution (mass fraction is75％～80％)
C1, dissolving the modified mixture T-C prepared in the step (2) in water at the temperature of 40 ℃ to obtain a solution a;
c2, adding CH to the solution a obtained in the step C13OCH3Carrying out precipitation reaction on the solution (the mass fraction is 80%), filtering after the reaction is finished, and keeping the precipitate;
c3 precipitation obtained in step C2 with anhydrous CH3CH2OH is washed for many times, then vacuum drying is carried out, the molecular weight is controlled to be 1000, and N, O carboxymethyl chitosan powder is obtained (substances with the molecular weight larger than 1000 can be returned to the step (2) to be mixed with the raw material chitosan for use (namely the mixed substances are used as chitosan), and the preparation of the modified mixture T-C is continuously carried out according to the step (2);
(4) preparation of mixture W
Raw materials (in parts by weight): 25 parts of white portland cement, 15 parts of modified mixture T-C and 0.1 part of N, O carboxymethyl chitosan;
uniformly mixing white portland cement, the modified mixture T-C obtained in the step (2) and the N, O carboxymethyl chitosan obtained in the step (3) according to the proportion, and controlling the screen residue of a 80-micron square-hole screen to be less than 1% to obtain a mixture W;
(5) preparation of finished product of colored dry-mixed mortar
Raw materials (in parts by weight): 90 parts of machine-made sand, 10 parts of mixture W, 10 parts of stone powder, 1 part of pigment (iron oxide yellow), 1 part of redispersible latex powder, 0.2 part of hydroxypropyl methyl cellulose ether and 15 parts of zeolite powder;
and uniformly mixing the machine-made sand, the mixture W, the stone powder, the pigment, the redispersible latex powder, the hydroxypropyl methyl cellulose ether and the zeolite powder according to the proportion to obtain a finished product of the color dry-mixed mortar.
Example 3:
preparing color dry-mixed mortar:
(1) preparing modified titanium dioxide:
raw materials (in parts by weight): 1 part of butyl titanate and 6 parts of water;
a1, adding butyl titanate into a reactor, and heating at 110 ℃ and N2Under the protection of titanium dioxideEster gasification;
a2, adding water into the reactor, reacting at 530 ℃ and 0.5 × 105Pa、N2Under the protection of (1L/min of nitrogen flow, 1L/min of water vapor flow and 20min of reaction time), obtaining R818 type nano TiO2；
A3, and the nanometer TiO obtained in the step A22Placing in inert gas CO2Cooling to 24 ℃ in the atmosphere;
a4, cooling the TiO obtained in the step A32Placing in a 45 μm round hole sieve, and controlling TiO2The content is more than 98 percent, the screen residue is less than 0.01 percent, the volatile matter at 105 ℃ is less than 0.05 percent, and the L value range is 98.5-100, thus obtaining the finished product of the modified titanium dioxide;
(2) preparation of modified mixture T-C
Raw materials (in parts by weight): 0.8 part of chitosan, 11 parts of isopropanol and ClCH21.2 parts of COOH and 85 parts of modified titanium dioxide;
b1, adding chitosan and a NaOH solution (the mass fraction is 58%) into a reaction container, wherein the mass ratio of the chitosan to the NaOH solution is 1:10, and the chitosan is alkalized in the NaOH solution;
b2, adding isopropanol and ClCH into the reaction vessel in sequence2COOH is stirred evenly and then placed for 2.8 hours at the temperature of 18 ℃; then heating to 68 ℃, and preserving heat for 1.6 h; then using CH3Adjusting the pH value to 6.5 by COOH;
b3, adding the modified titanium dioxide prepared in the step (1) into a reaction container, uniformly stirring to obtain a mixture, filtering the mixture, and keeping a precipitate;
b4, using CH in turn for the precipitate obtained in the step B33CH2Washing with OH solution (mass fraction of 62%) and anhydrous methanol;
b5, drying at the temperature of 55 ℃ after washing to obtain a modified mixture T-C;
(3) preparation of N, O carboxymethyl chitosan
Raw materials (in parts by weight): modified mixture T-C, water, CH3OCH3Solution (mass fraction is 75% -80%)
C1, dissolving the modified mixture T-C prepared in the step (2) in water at the temperature of 32 ℃ to obtain a solution a;
c2, adding CH to the solution a obtained in the step C13OCH3Carrying out precipitation reaction on the solution (the mass fraction is 76%), filtering after the reaction is finished, and keeping the precipitate;
c3 precipitation obtained in step C2 with anhydrous CH3CH2OH is washed for many times, then vacuum drying is carried out, the molecular weight is controlled to be 10000, and N, O carboxymethyl chitosan powder is obtained (substances with the molecular weight larger than 10000 can be returned to the step (2) to be mixed with the raw material chitosan for use (namely the mixed substances are used as chitosan), and the preparation of the modified mixture T-C is continuously carried out according to the step (2);
(4) preparation of mixture W
Raw materials (in parts by weight): 22 parts of white portland cement, 14 parts of modified mixture T-C and 0.2 part of N, O carboxymethyl chitosan;
uniformly mixing white portland cement, the modified mixture T-C obtained in the step (2) and the N, O carboxymethyl chitosan obtained in the step (3) according to the proportion, and controlling the screen residue of a 80-micron square-hole screen to be less than 1% to obtain a mixture W;
(5) preparation of finished product of colored dry-mixed mortar
Raw materials (in parts by weight): 82 parts of machine-made sand, 12 parts of mixture W, 8 parts of stone powder, 4 parts of pigment (iron oxide green), 0.3 part of redispersible latex powder, 1 part of hydroxypropyl methyl cellulose ether and 14 parts of zeolite powder;
and uniformly mixing the machine-made sand, the mixture W, the stone powder, the pigment, the redispersible latex powder, the hydroxypropyl methyl cellulose ether and the zeolite powder according to the proportion to obtain a finished product of the color dry-mixed mortar.
Example 4:
preparing color dry-mixed mortar:
(1) preparing modified titanium dioxide:
raw materials (in parts by weight): 1 part of butyl titanate and 20 parts of water;
a1, adding butyl titanate into a reactor, and heating at 130 ℃ and N2Under protection, butyl titanate is gasified;
a2, mixingWater is added into the reactor at a reaction temperature of 550 ℃ and a pressure of 1.2 × 105Pa、N2Under the protection of (1.2L/min nitrogen flow, 1.2L/min water vapor flow, 35min reaction time), to obtain R818 type nanometer TiO2；
A3, and the nanometer TiO obtained in the step A22Placing in inert gas CO2Cooling to 25 ℃ in the atmosphere;
a4, cooling the TiO obtained in the step A32Placing in a 45 μm round hole sieve, and controlling TiO2The content is more than 98 percent, the screen residue is less than 0.01 percent, the volatile matter at 105 ℃ is less than 0.05 percent, and the L value range is 98.5-100, thus obtaining the finished product of the modified titanium dioxide;
(2) preparation of modified mixture T-C
Raw materials (in parts by weight): 1.2 parts of chitosan, 9 parts of isopropanol and ClCH21.8 parts of COOH and 86 parts of modified titanium dioxide;
b1, adding chitosan and a NaOH solution (the mass fraction is 52%) into a reaction container, wherein the mass ratio of the chitosan to the NaOH solution is 1:12, and the chitosan is alkalized in the NaOH solution;
b2, adding isopropanol and ClCH into the reaction vessel in sequence2COOH is stirred evenly and then placed for 2.2 hours at the temperature of 22 ℃; then heating to 66 ℃, and preserving heat for 1.8 h; then using CH3Adjusting the pH value to 7.5 by COOH;
b3, adding the modified titanium dioxide prepared in the step (1) into a reaction container, uniformly stirring to obtain a mixture, filtering the mixture, and keeping a precipitate;
b4, using CH in turn for the precipitate obtained in the step B33CH2Washing with OH solution (68% by mass) and anhydrous methanol;
b5, drying at the temperature of 65 ℃ after washing to obtain a modified mixture T-C;
(3) preparation of N, O carboxymethyl chitosan
Raw materials (in parts by weight): modified mixture T-C, water, CH3OCH3Solution (mass fraction is 75% -80%)
C1, dissolving the modified mixture T-C prepared in the step (2) in water at the temperature of 38 ℃ to obtain a solution a;
c2, adding CH to the solution a obtained in the step C13OCH3Carrying out precipitation reaction on the solution (the mass fraction is 78%), filtering after the reaction is finished, and keeping the precipitate;
c3 precipitation obtained in step C2 with anhydrous CH3CH2OH washing (for many times), then vacuum drying, controlling the molecular weight to be 40000, obtaining N, O carboxymethyl chitosan powder (substances with the molecular weight larger than 40000 can be returned to the step (2) to be mixed with the raw material chitosan for use (namely, the mixed substances are used as chitosan), and the preparation of the modified mixture T-C is continuously carried out according to the step (2);
(4) preparation of mixture W
Raw materials (in parts by weight): 24 parts of white portland cement, 11 parts of modified mixture T-C and 0.4 part of N, O carboxymethyl chitosan;
uniformly mixing white portland cement, the modified mixture T-C obtained in the step (2) and the N, O carboxymethyl chitosan obtained in the step (3) according to the proportion, and controlling the screen residue of a 80-micron square-hole screen to be less than 1% to obtain a mixture W;
(5) preparation of finished product of colored dry-mixed mortar
Raw materials (in parts by weight): 88 parts of machine-made sand, 14 parts of mixture W, 3 parts of stone powder, 2 parts of pigment, 0.8 part of redispersible latex powder, 0.4 part of hydroxypropyl methyl cellulose ether and 11 parts of zeolite powder;
and uniformly mixing the machine-made sand, the mixture W, the stone powder, the pigment, the redispersible latex powder, the hydroxypropyl methyl cellulose ether and the zeolite powder according to the proportion to obtain a finished product of the color dry-mixed mortar.
Example 5:
preparing color dry-mixed mortar:
(1) preparing modified titanium dioxide:
raw materials (in parts by weight): 1 part of butyl titanate and 2 parts of water;
a1, adding butyl titanate into a reactor at 40 ℃ and N2Under protection, butyl titanate is gasified;
a2, adding water into the reactor, reacting at 500 deg.C and 0.8 × 105Pa、N2Under the protection of (nitrogen flow is 0.5L/min, water vapor flow is 2.0L/min, reaction time is 20min) to obtain R818 type nano TiO2；
A3, and the nanometer TiO obtained in the step A22Placing in inert gas CO2Cooling to 20 ℃ in the atmosphere;
a4, cooling the TiO obtained in the step A32Placing in a 45 μm round hole sieve, and controlling TiO2The content is more than 98 percent, the screen residue is less than 0.01 percent, the volatile matter at 105 ℃ is less than 0.05 percent, and the L value range is 98.5-100, thus obtaining the finished product of the modified titanium dioxide;
(2) preparation of modified mixture T-C
Raw materials (in parts by weight): 1 part of chitosan, 10 parts of isopropanol and ClCH21.5 parts of COOH and 88 parts of modified titanium dioxide;
b1, adding chitosan and a NaOH solution (the mass fraction is 50-60%) into a reaction container, wherein the mass ratio of the chitosan to the NaOH solution is 1:14, and the chitosan is alkalized in the NaOH solution;
b2, adding isopropanol and ClCH into the reaction vessel in sequence2COOH is stirred evenly and then placed for 1.5 hours at the temperature of 20 ℃; then heating to 67 ℃, and preserving heat for 1.8 h; then using CH3Adjusting the PH value to 7 by COOH;
b3, adding the modified titanium dioxide prepared in the step (1) into a reaction container, uniformly stirring to obtain a mixture, filtering the mixture, and keeping a precipitate;
b4, using CH in turn for the precipitate obtained in the step B33CH2Washing with OH solution (65% by weight) and anhydrous methanol;
b5, drying at the temperature of 60 ℃ after washing to obtain a modified mixture T-C;
(3) preparation of N, O carboxymethyl chitosan
Raw materials (in parts by weight): modified mixture T-C, water, CH3OCH3Solution (mass fraction is 75% -80%)
C1, dissolving the modified mixture T-C prepared in the step (2) in water with the temperature of 35 ℃ to obtain a solution a;
c2, adding CH to the solution a obtained in the step C13OCH3Carrying out precipitation reaction on the solution (the mass fraction is 77%), filtering after the reaction is finished, and keeping the precipitate;
c3 precipitation obtained in step C2 with anhydrous CH3CH2OH washing (for many times), then vacuum drying, controlling the molecular weight to be 30000, obtaining N, O carboxymethyl chitosan powder (substances with the molecular weight larger than 30000 can be returned to the step (2) to be mixed with the raw material chitosan for use (namely, the mixed substances are used as chitosan), and the preparation of the modified mixture T-C is continuously carried out according to the step (2));
(4) preparation of mixture W
Raw materials (in parts by weight): 23 parts of white portland cement, 12 parts of modified mixture T-C and 0.3 part of N, O carboxymethyl chitosan;
uniformly mixing white portland cement, the modified mixture T-C obtained in the step (2) and the N, O carboxymethyl chitosan obtained in the step (3) according to the proportion, and controlling the screen residue of a 80-micron square-hole screen to be less than 1% to obtain a mixture W;
(5) preparation of finished product of colored dry-mixed mortar
Raw materials (in parts by weight): 85 parts of machine-made sand, 12 parts of mixture W, 6 parts of stone powder, 3 parts of pigment (iron oxide red), 0.5 part of redispersible latex powder, 0.8 part of hydroxypropyl methyl cellulose ether and 12 parts of zeolite powder;
and uniformly mixing the machine-made sand, the mixture W, the stone powder, the pigment, the redispersible latex powder, the hydroxypropyl methyl cellulose ether and the zeolite powder according to the proportion to obtain a finished product of the color dry-mixed mortar.
Second, Experimental example
The colored dry-mixed mortars prepared in examples 1 to 5 were subjected to construction:
1. preparing cement mortar:
water was added directly to the colored dry-mixed mortar prepared in example 1, and the added water was added in a weight ratio (colored dry-mixed mortar: water: 150: 1000);
water was directly added to the colored dry-mixed mortar prepared in example 2, and the added water was added in a weight ratio (colored dry-mixed mortar: water: 200: 1000);
water was added directly to the colored dry-mixed mortar prepared in example 3, and the added water was added in a weight ratio (colored dry-mixed mortar: water: 165: 1000);
water was added directly to the colored dry-mixed mortar prepared in example 4, the added water being added in a weight ratio (colored dry-mixed mortar: water 185: 1000);
water was added directly to the colored dry-mixed mortar prepared in example 5, and the added water was added in a weight ratio (colored dry-mixed mortar: water: 175: 1000);
2. construction:
during construction, if the construction is carried out according to the traditional color mortar, the wall surface must be coated with finish paint before construction, but the color dry-mixed mortar prepared in the embodiments 1 to 5 of the invention has the functions of water resistance and saltpetering resistance, can be directly primed and plastered according to the operation of the traditional plastering mortar, is extremely convenient to construct, can reduce two construction procedures (a finish paint coating procedure and a bottom layer plastering mortar procedure) during construction, and can improve the construction efficiency by 200 percent.
The cement mortar prepared from the color dry-mixed mortar prepared in the embodiments 1 to 5 has good workability and convenient consistency adjustment, when the mortar consistency is 90mm to 100mm, the color of the mortar construction wall surface is bright, the color main body can still be well expressed in a wet state, and the bleeding phenomenon does not occur in the construction;
the colored dry-mixed mortar prepared in the examples 1 to 5 and the colored mortar (stuccoo color mortar produced by Chengdu Leili paint particle Co., Ltd.) in the prior art are used as comparative examples, construction is carried out under the same conditions, the performance after construction is tested according to GB 50210-:
the cement mortar prepared from the color dry-mixed mortar prepared in the examples 1 to 5 has good cohesiveness and smooth and soft plastering surface.
TABLE 1 construction Properties comparison Table
As can be seen from table 1:
the compressive strength of the color dry-mixed mortar prepared in the examples 1 to 5 after 7d is higher than that of the color mortar prepared in the comparative example under the same conditions;
the color dry-mixed mortar prepared in the embodiments 1 to 5 has no obvious difference between the wall color at 28d and the wall color at 3d, because the color dry-mixed mortar prepared in the embodiments 1 to 5 of the invention basically does not absorb water after 1 hour, and the surface moisture evaporates quickly; whereas the wall in the comparative example turned white in color.
③ the compression strength and the tensile strength of the color dry-mixed mortar prepared in the examples 1 to 5 are not changed from the dry-mixed mortar in the comparative example, the weather resistance is improved by 50 to 100 percent, the phenomena of saltpetering, powder falling and hollowing cracking are avoided, the pollution resistance is obviously improved, and the grade 1 is achieved.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention.
Claims (10)
1. A color dry-mixed mortar is characterized in that: the preparation comprises the following components in parts by weight:
80-90 parts of machine-made sand;
10-15 parts of a mixture W;
1-10 parts of stone powder;
1-5 parts of pigment;
0.1 to 1 portion of redispersible latex powder;
0.2 to 1.2 portions of hydroxypropyl methyl cellulose ether;
10-15 parts of zeolite powder;
the mixture W is prepared from white portland cement, a modified mixture T-C and N, O carboxymethyl chitosan; the weight percentage content of calcium oxide in the white portland cement is 58-65%;
the modified mixture T-C consists of a shellGlycan, isopropanol, ClCH2COOH and modified titanium dioxide.
2. The colored dry-mixed mortar of claim 1, wherein: the weight parts of each component are respectively as follows:
82-88 parts of machine-made sand;
12-14 parts of a mixture W;
3 to 8 portions of stone powder,
2-4 parts of pigment;
0.3 to 0.8 portion of redispersible latex powder;
0.4 to 1 part of hydroxypropyl methyl cellulose ether;
11 to 14 portions of zeolite powder.
3. The colored dry-mixed mortar according to claim 2, wherein: the weight parts of each component are respectively as follows:
85 parts of machine-made sand;
12 parts of a mixture W;
6 parts of stone powder, namely 6 parts of stone powder,
3 parts of a pigment;
0.5 part of redispersible latex powder;
0.8 part of hydroxypropyl methyl cellulose ether;
12 parts of zeolite powder.
4. The color dry-mixed mortar according to any one of claims 1 to 3, wherein: the preparation of the mixture W comprises the following raw materials in parts by weight:
20-25 parts of white portland cement;
10-15 parts of modified mixture T-C;
0.1 to 0.5 portion of N, O carboxymethyl chitosan.
5. The colored dry-mixed mortar of claim 4, wherein: the preparation of the mixture W comprises the following raw materials in parts by weight:
22-24 parts of white portland cement;
11-14 parts of modified mixture T-C;
0.2 to 0.4 portion of N, O carboxymethyl chitosan.
6. The color dry-mixed mortar according to any one of claims 1 to 3, wherein: the modified mixture T-C is prepared from the following raw materials in parts by weight:
0.5-1.5 parts of chitosan;
8-12 parts of isopropanol;
ClCH21-2 parts of COOH;
85-90 parts of modified titanium dioxide.
7. The colored dry-mixed mortar of claim 6, wherein: the modified mixture T-C is prepared from the following raw materials in parts by weight:
1 part of chitosan
10 portions of isopropanol
ClCH2COOH 1.5 parts
87 parts of modified titanium dioxide.
8. The method for preparing the color dry-mixed mortar according to any one of claims 1 to 7, wherein the method comprises the following steps: the method comprises the following steps:
(1) preparation of modified titanium white powder
A1, adding butyl titanate into a reactor, and gasifying the butyl titanate at the temperature of 40-130 ℃ under the protection of inert gas;
a2, adding water into a reactor, reacting at 500-550 ℃ and 0.5 × 105Pa～1.5×105Pa, inert gas protection to obtain nano TiO2；
A3, and the nanometer TiO obtained in the step A22Placing the mixture in an inert gas atmosphere to reduce the temperature to 20-25 ℃;
a4, cooling the TiO obtained in the step A32Carrying out screen analysis to obtain a finished product of the modified titanium dioxide;
(2) preparation of modified mixture T-C
B1, adding chitosan and NaOH solution into a reaction container, and alkalizing the chitosan in the NaOH solution;
b2, adding isopropanol and ClCH into the reaction vessel in sequence2COOH is evenly stirred and then is placed for 2 to 3 hours at the temperature of between 15 and 25 ℃; then heating to 65-70 ℃, and preserving the heat for 1.5-2 h; then adjusting the pH value to 6-8;
b3, adding the modified titanium dioxide prepared in the step (1) into a reaction container, uniformly stirring to obtain a mixture, filtering the mixture, and keeping a precipitate;
b4, using CH in turn for the precipitate obtained in the step B33CH2Washing with OH solution and anhydrous methanol;
b5, drying at 50-70 ℃ after washing to obtain a modified mixture T-C;
(3) preparation of N, O carboxymethyl chitosan
C1, dissolving the modified mixture T-C prepared in the step (2) in water at the temperature of 30-40 ℃ to obtain a solution a;
c2, adding CH to the solution a obtained in the step C13OCH3Carrying out precipitation reaction on the solution, filtering after the reaction is finished, and keeping the precipitate;
c3 precipitation obtained in step C2 with anhydrous CH3CH2OH washing, and then vacuum drying to obtain N, O carboxymethyl chitosan powder;
(4) preparation of mixture W
Uniformly mixing white portland cement, the modified mixture T-C obtained in the step (2) and the N, O carboxymethyl chitosan obtained in the step (3) according to a ratio to obtain a mixture W;
(5) preparation of finished product of colored dry-mixed mortar
And uniformly mixing the machine-made sand, the mixture W, the stone powder, the pigment, the redispersible latex powder, the hydroxypropyl methyl cellulose ether and the zeolite powder according to the proportion to obtain a finished product of the color dry-mixed mortar.
9. The method for preparing a colored dry-mixed mortar according to claim 8, wherein: in the step (1) A4, the screening is to be performedCooling the TiO obtained in step (1) A32Placing in a 45 μm round hole sieve, and controlling TiO2The content is more than 98%, the screen residue is less than 0.01%, the volatile matter at 105 ℃ is less than 0.05%, and the L value range is 98.5-100.
10. The method for preparing a colored dry-mixed mortar according to claim 8 or 9, wherein: in the step (1) A2, the mass ratio of the water to the butyl titanate is 2: 1-20: 1.
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