Background
The bottom plastering gypsum is prepared by taking semi-hydrated gypsum as a main cementing material, adding light aggregate and an additive and mixing, is widely applied to wall plastering in construction engineering, and is a building material widely used in construction engineering. The bottom layer plastering gypsum has the following advantages: (1) The bottom layer plastering gypsum is used as A1-grade non-combustible material, and has excellent heat preservation, heat insulation, sound insulation and fire resistance; (2) The mortar has strong binding power, is not easy to fall off, has small contractibility, overcomes the phenomena of hollowing and cracking which often occur in the traditional cement mortar, and basically avoids the common defects of plastering quality; and (3) the workability is good. The paint does not bleed or separate, is convenient to construct, can be directly used by adding water, and has simple and convenient working procedures; less falling ash, quick operation and short operation time. The coagulation time can be adjusted according to the needs; (4) The water-retaining agent has good water-retaining property and workability, is used for walls with strong water absorption capacity such as aerated concrete and the like, can ensure complete hydration reaction after plastering, and can prevent the strength of a plastering layer from being reduced due to water loss. Interface treatment is not needed for various wall surfaces such as concrete, aerated concrete and the like, and the wall surfaces can be directly used, so that the engineering cost is effectively saved; and (5) construction period is saved. The bottom layer plastering gypsum can survive once, and because the strength of the bottom layer plastering gypsum is increased quickly and is easy to dry, a plurality of working procedures can be saved, the construction progress is accelerated, and the bottom layer plastering gypsum is suitable for projects with large plastering workload and short construction period. Because the bottom layer plastering gypsum has the advantages, the method is widely researched.
The patent with the application number of 202110136295.5 discloses bottom layer plastering gypsum and a preparation method thereof, and the bottom layer plastering gypsum patent meeting the relevant performance requirements of GB/T28627-2012 plastering gypsum is prepared by taking desulfurized building gypsum, semidry desulfurized fly ash and fine aggregates as raw materials, taking a composite retarder, a water-retaining agent and starch ether as additives and adjusting the composite retarder proportion and the bottom layer plastering gypsum formula. The patent with the application number of 201910259761.1 discloses a lightweight bottom layer plastering gypsum mortar, which comprises the following components in parts by weight: 477 parts of desulfurized gypsum; 332-470 parts of fly ash; 8-12 parts of artificial machine-made fine sand; 40-180 parts of closed-cell vitrified micro-beads; 1 part of rubber powder; 1-2 parts of retarder; and 2 parts of a water retaining agent. The lightweight bottom layer plastering gypsum mortar utilizes wastes of thermal power generation, and can well reduce pollution. The patent with the application number of 202011328060.8 discloses a regeneration building bottom layer plastering gypsum and a preparation method thereof, and the regeneration building bottom layer plastering gypsum comprises 100-200 parts of salt gypsum, 10-20 parts of a dissolution promoter and 50-60 parts of an enhancing additive, wherein the dissolution promoter comprises heptasodium diethylenetriamine penta (methylene phosphonic acid), potassium formate and zeolite powder, wherein the mass ratio of the heptasodium diethylenetriamine penta (methylene phosphonic acid), the potassium formate and the zeolite powder is 1:2: the reinforcing admixture comprises a retarder, latex powder, a water reducing agent, portland cement, vitrified micro bubbles and diatomite, wherein the mass of the Portland cement is 50-60% of that of the reinforcing admixture. From the prior art, most of the existing researches on the bottom plastering gypsum reduce the preparation cost, but the functional researches on the bottom plastering gypsum are less.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the invention provides the bottom layer plastering gypsum and the preparation method thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a preparation method of bottom layer plastering gypsum comprises the following steps:
(1) Mixing paraffin and tetrabutyl titanate, adding the mixture into a mixed solution of deionized water and absolute ethyl alcohol, adding hexadecyl trimethyl ammonium bromide, stirring at a high speed to prepare an emulsion, slowly dropwise adding ammonia water into the emulsion while stirring, continuing stirring for reaction after the dropwise adding is finished, filtering after the reaction is finished, and drying the solid to prepare the single-shell microcapsule;
(2) Adding the prepared single-shell microcapsule into a Tris-HCl buffer solution with the pH value of 8.5, carrying out ultrasonic treatment, then adding dopamine, carrying out stirring reaction, filtering after the reaction is finished, and drying the solid obtained by filtering to obtain a double-shell phase-change material;
(3) And (3) premixing the desulfurized gypsum, the cement, the sand, the double-shell phase-change material and the redispersible latex powder, adding the water-retaining agent and the retarder, and uniformly stirring and mixing to prepare the bottom layer plastering gypsum.
Preferably, in the step (1), the mass ratio of the paraffin, tetrabutyl titanate and hexadecyl trimethyl ammonium bromide is 15: (10-15): (1-2).
Preferably, in the step (1), the volume ratio of the deionized water to the absolute ethyl alcohol in the mixed solution is (2-2.5): 1.
preferably, in the step (1), the rotation speed of the high-speed stirring treatment is 15000-20000rpm, and the time of the high-speed stirring treatment is 3-8min.
Preferably, in the step (1), the mass concentration of the ammonia water is 25wt%, and the dosage ratio of the ammonia water to the tetrabutyl titanate is (2-3) ml:10g, and the dropping speed of the ammonia water is 1ml/min.
Preferably, in the step (1), the temperature of the reaction system is maintained at 60 to 70 ℃ while dropping the aqueous ammonia, the stirring speed is 300 to 400rpm, and the stirring reaction time after completion of the dropping is 4 to 5 hours.
Preferably, in the step (2), the addition amount of the dopamine is 0.5 to 2 percent of the mass of the tetrabutyl titanate; the concentration of the dopamine in a Tris-HCl buffer solution is 0.5-2g/L.
Preferably, in the step (3), the amounts of the components are as follows in parts by weight: 100 parts of desulfurized gypsum, 5-10 parts of cement, 30-50 parts of sand, 10-20 parts of double-shell phase-change material, 10-20 parts of redispersible latex powder, 10-20 parts of water-retaining agent and 1.5-10 parts of retarder.
Preferably, in the step (3), the rotation speed of the premixing treatment is 300-500rpm, the time is 3-5min, and the rotation speed of the stirring and mixing is 800-1000rpm, and the time is 10-20min.
Preferably, in the step (3), the purity of the desulfurized gypsum is more than or equal to 80%, the fineness modulus of the sand is 1.9, the water-retaining agent is hydroxypropyl methylcellulose, and the retarder is sodium citrate.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
the bottom layer plastering gypsum provided by the invention comprises desulfurized gypsum, sand, a double-shell phase-change material, redispersible latex powder, a water-retaining agent and a retarder, wherein hydroxypropyl methyl cellulose ether is used as the water-retaining agent, sodium citrate is used as the retarder, the redispersible latex powder is added as a binder, and the self-made double-shell phase-change material is added for modification, so that the prepared bottom layer plastering gypsum has excellent heat insulation performance and the strength is not obviously reduced.
The double-shell phase-change material prepared by the invention takes paraffin as a phase-change active component, firstly coats titanium oxide on the surface of the paraffin, and then coats a poly-dopamine layer on the surface of the paraffin to form a double-shell structure, so that the leakage of the phase-change active component in the phase-change material can be effectively prevented, and the stability of the phase-change material is improved. The method effectively controls the dosage of dopamine, thereby improving the roughness of the surface of the microcapsule and further improving the interface performance of the phase change material and the gypsum matrix, the surface of the double-shell phase change material prepared after poly-dopamine coating has certain roughness, the interface friction between the double-shell phase change material and the gypsum matrix is increased, the interlocking effect improves the interface performance of the phase change material and the matrix, and the heat insulation performance of the plastering gypsum is improved on the premise of not influencing the strength of the matrix.
Detailed Description
The invention is further illustrated by the following examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1
(1) Mixing 15g of paraffin and 10g of tetrabutyl titanate, adding the mixture into a mixed solution of 100ml of deionized water and 50ml of absolute ethyl alcohol, then adding 1g of hexadecyl trimethyl ammonium bromide, stirring at a high speed of 15000rpm for 5min to prepare an emulsion, heating to 60 ℃, then dropwise adding 2ml of 25wt% ammonia water into the emulsion at a dropwise adding speed of 1ml/min, stirring while dropwise adding, controlling the stirring speed to be 300rpm, continuously stirring for reacting for 4h after dropwise adding, filtering after the reaction is finished, drying the solid, and preparing the single-shell microcapsule;
(2) Adding the prepared single-shell microcapsule into 100ml of Tris-HCl buffer solution with the pH value of 8.5, carrying out ultrasonic treatment, then adding 0.2g of dopamine, carrying out stirring reaction for 30min, filtering after the reaction is finished, and drying the solid obtained by filtering to obtain the double-shell phase-change material;
(3) The method comprises the following steps of premixing 100 parts by weight of desulfurized gypsum, 10 parts by weight of cement, 30 parts by weight of sand, 15 parts by weight of double-shell phase change material and 15 parts by weight of redispersible latex powder at the rotating speed of 300rpm for 3min, then adding 15 parts by weight of hydroxypropyl methylcellulose and 8 parts by weight of sodium citrate, and stirring and mixing at the rotating speed of 800rpm for 10min to obtain the bottom layer plastering gypsum.
Example 2
(1) Mixing 15g of paraffin and 10g of tetrabutyl titanate, adding the mixture into a mixed solution of 100ml of deionized water and 50ml of absolute ethyl alcohol, then adding 2g of hexadecyl trimethyl ammonium bromide, stirring at a high speed of 20000rpm for 8min to prepare an emulsion, heating to 70 ℃, then dropwise adding 3ml of 25wt% ammonia water into the emulsion at a dropwise adding speed of 1ml/min, stirring while dropwise adding, controlling the stirring speed to be 400rpm, continuously stirring for reacting for 5h after the dropwise adding is finished, filtering after the reaction is finished, drying the solid, and preparing the single-shell microcapsule;
(2) Adding the prepared single-shell microcapsule into 100ml of Tris-HCl buffer solution with the pH value of 8.5, carrying out ultrasonic treatment, then adding 0.2g of dopamine, carrying out stirring reaction for 30min, filtering after the reaction is finished, and drying the solid obtained by filtering to obtain a double-shell phase-change material;
(3) The method comprises the following steps of premixing 100 parts by weight of desulfurized gypsum, 10 parts by weight of cement, 45 parts by weight of sand, 15 parts by weight of double-shell phase change material and 15 parts by weight of redispersible latex powder at the rotating speed of 500rpm for 5min, then adding 15 parts by weight of hydroxypropyl methylcellulose and 10 parts by weight of sodium citrate, and stirring and mixing at the rotating speed of 1000rpm for 20min to obtain the bottom layer plastering gypsum.
Example 3
(1) Mixing 15g of paraffin and 10g of tetrabutyl titanate, adding the mixture into a mixed solution of 100ml of deionized water and 50ml of absolute ethyl alcohol, then adding 1.5g of hexadecyl trimethyl ammonium bromide, stirring at a high speed of 15000rpm for 8min to prepare an emulsion, heating to 65 ℃, then dropwise adding 3ml of 25wt% ammonia water into the emulsion at a dropwise adding speed of 1ml/min, stirring while dropwise adding, controlling the stirring speed to be 400rpm, continuously stirring for reacting for 4h after the dropwise adding is finished, filtering after the reaction is finished, drying the solid, and preparing the single-shell microcapsule;
(2) Adding the prepared single-shell microcapsule into 100ml of Tris-HCl buffer solution with the pH value of 8.5, carrying out ultrasonic treatment, then adding 0.15g of dopamine, carrying out stirring reaction for 30min, filtering after the reaction is finished, and drying the solid obtained by filtering to obtain the double-shell phase-change material;
(3) The method comprises the following steps of premixing 100 parts by weight of desulfurized gypsum, 10 parts by weight of cement, 50 parts by weight of sand, 15 parts by weight of double-shell phase change material and 15 parts by weight of redispersible latex powder at the rotating speed of 350rpm for 3min, then adding 15 parts by weight of hydroxypropyl methylcellulose and 8 parts by weight of sodium citrate, and stirring and mixing at the rotating speed of 850rpm for 10min to obtain the bottom layer plastering gypsum.
Example 4
(1) Mixing 15g of paraffin and 10g of tetrabutyl titanate, adding the mixture into a mixed solution of 100ml of deionized water and 50ml of absolute ethyl alcohol, then adding 1.5g of hexadecyl trimethyl ammonium bromide, stirring at a high speed of 20000rpm for 3min to prepare an emulsion, heating to 60 ℃, then dropwise adding 3ml of 25wt% ammonia water into the emulsion at a dropwise adding speed of 1ml/min, stirring while dropwise adding, controlling the stirring speed to 350rpm, continuously stirring for reacting for 4h after the dropwise adding is finished, filtering after the reaction is finished, drying the solid, and preparing the single-shell microcapsule;
(2) Adding the prepared single-shell microcapsule into 100ml of Tris-HCl buffer solution with the pH value of 8.5, carrying out ultrasonic treatment, then adding 0.2g of dopamine, carrying out stirring reaction for 30min, filtering after the reaction is finished, and drying the solid obtained by filtering to obtain the double-shell phase-change material;
(3) The method comprises the following steps of premixing 100 parts by weight of desulfurized gypsum, 10 parts by weight of cement, 45 parts by weight of sand, 15 parts by weight of double-shell phase change material and 15 parts by weight of redispersible latex powder at the rotating speed of 400rpm for 3min, then adding 108 parts by weight of hydroxypropyl methylcellulose and 8 parts by weight of sodium citrate, and stirring and mixing at the rotating speed of 900rpm for 120min to obtain the bottom layer plastering gypsum.
Example 5
(1) Mixing 15g of paraffin and 10g of tetrabutyl titanate, adding the mixture into a mixed solution of 100ml of deionized water and 50ml of absolute ethyl alcohol, then adding 2g of hexadecyl trimethyl ammonium bromide, stirring at a high speed of 15000rpm for 8min to prepare an emulsion, heating to 65 ℃, then dropwise adding 3ml of 25wt% ammonia water into the emulsion at a dropwise adding speed of 1ml/min, stirring while dropwise adding, controlling the stirring speed to be 300rpm, continuously stirring for reacting for 5h after dropwise adding, filtering after the reaction is finished, drying the solid, and preparing the single-shell microcapsule;
(2) Adding the prepared single-shell microcapsule into 100ml of Tris-HCl buffer solution with the pH value of 8.5, carrying out ultrasonic treatment, then adding 0.2g of dopamine, carrying out stirring reaction for 30min, filtering after the reaction is finished, and drying the solid obtained by filtering to obtain the double-shell phase-change material;
(3) The method comprises the following steps of premixing 100 parts by weight of desulfurized gypsum, 10 parts by weight of cement, 48 parts by weight of sand, 15 parts by weight of double-shell phase change material and 15 parts by weight of redispersible latex powder at the rotating speed of 450rpm for 5min, then adding 15 parts by weight of hydroxypropyl methylcellulose and 8 parts by weight of sodium citrate, and stirring and mixing at the rotating speed of 950rpm for 20min to obtain the bottom layer plastering gypsum.
Comparative example 1
The phase change material was not coated with polydopamine, and the other conditions were the same as in example 5.
The performance tests were carried out on the plasters prepared in the above examples and comparative examples, and the test results and test methods were as follows:
mechanical properties of the gypsum sample are molded and maintained according to related regulations of JC/T1023-2021 gypsum-based self-leveling mortar, and the mechanical properties, setting time and fluidity of the gypsum sample are tested after drying and cooling.
The heat conductivity coefficient of the plastering gypsum is respectively measured according to GB/T10294-2008 ' method for measuring the steady-state thermal resistance and related characteristics of the antipyretic material's heat shield plate ' and JGJ51-2002 ' technical code of lightweight aggregate concrete '.
TABLE 1
The test results show that when the phase change material is coated with the polydopamine for the second time, the heat preservation performance of the bottom layer plastering gypsum is improved, and the mechanical performance of the bottom layer plastering gypsum is also improved, mainly because the surface of the single-shell microcapsule formed by the titanium dioxide coated paraffin is smooth and has poor interface performance with a matrix, but after the polydopamine is coated, the surface roughness of the phase change material is increased, and the polydopamine has certain adhesion to an inorganic matrix, so that the interface performance of the phase change material and the matrix is effectively improved.
Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.