CN116218276B - Interior wall smooth putty powder - Google Patents
Interior wall smooth putty powder Download PDFInfo
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- CN116218276B CN116218276B CN202310408052.1A CN202310408052A CN116218276B CN 116218276 B CN116218276 B CN 116218276B CN 202310408052 A CN202310408052 A CN 202310408052A CN 116218276 B CN116218276 B CN 116218276B
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- guar gum
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- silicone oil
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- 239000000843 powder Substances 0.000 title claims abstract description 70
- 229920002545 silicone oil Polymers 0.000 claims abstract description 58
- 229920002907 Guar gum Polymers 0.000 claims abstract description 54
- 239000000665 guar gum Substances 0.000 claims abstract description 54
- 235000010417 guar gum Nutrition 0.000 claims abstract description 54
- 229960002154 guar gum Drugs 0.000 claims abstract description 54
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 51
- 229920000570 polyether Polymers 0.000 claims abstract description 51
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 19
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 19
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 19
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 19
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 19
- 229960004853 betadex Drugs 0.000 claims abstract description 19
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 19
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 19
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 19
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 19
- RQFQJYYMBWVMQG-IXDPLRRUSA-N chitotriose Chemical compound O[C@@H]1[C@@H](N)[C@H](O)O[C@H](CO)[C@H]1O[C@H]1[C@H](N)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)N)[C@@H](CO)O1 RQFQJYYMBWVMQG-IXDPLRRUSA-N 0.000 claims abstract description 19
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- 239000010440 gypsum Substances 0.000 claims abstract description 19
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 19
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 19
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 19
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 19
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 15
- 239000003607 modifier Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 216
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 147
- 239000000203 mixture Substances 0.000 claims description 119
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 61
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 56
- 238000003756 stirring Methods 0.000 claims description 54
- 239000007790 solid phase Substances 0.000 claims description 48
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 47
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 41
- 238000004321 preservation Methods 0.000 claims description 36
- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 claims description 35
- 239000012346 acetyl chloride Substances 0.000 claims description 35
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 29
- GAWAYYRQGQZKCR-UHFFFAOYSA-N 2-chloropropionic acid Chemical compound CC(Cl)C(O)=O GAWAYYRQGQZKCR-UHFFFAOYSA-N 0.000 claims description 28
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 28
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 28
- 229940116298 l- malic acid Drugs 0.000 claims description 28
- 235000011090 malic acid Nutrition 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 27
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 229960002989 glutamic acid Drugs 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- 239000004593 Epoxy Substances 0.000 claims description 17
- 239000012300 argon atmosphere Substances 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 230000003113 alkalizing effect Effects 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 230000003449 preventive effect Effects 0.000 claims description 6
- 239000013530 defoamer Substances 0.000 claims description 4
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims 1
- 239000006104 solid solution Substances 0.000 claims 1
- 239000003112 inhibitor Substances 0.000 abstract description 13
- 238000010276 construction Methods 0.000 abstract description 6
- 238000012423 maintenance Methods 0.000 abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 235000013312 flour Nutrition 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 6
- 244000303965 Cyamopsis psoralioides Species 0.000 description 5
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/34—Filling pastes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
- C08B37/0096—Guar, guar gum, guar flour, guaran, i.e. (beta-1,4) linked D-mannose units in the main chain branched with D-galactose units in (alpha-1,6), e.g. from Cyamopsis Tetragonolobus; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Wood Science & Technology (AREA)
- Emergency Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses interior wall smooth putty powder which comprises the components of desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methyl cellulose ether, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum modifier, carboxymethyl cellulose, sodium fluosilicate, dispersing agent, defoaming agent and mildew inhibitor; the putty powder has good bonding strength and water resistance, improves the service performance of the interior wall putty powder, is not easy to fall off or crack after construction, prolongs the service life, and reduces the maintenance cost of the wall.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to interior wall smooth putty powder.
Background
The structure of modern architecture is an organic whole, and the bearing wall body, the functional heat preservation layer, the waterproof layer and the decorative layer are mutually complemented by each other, which is indispensable. The putty is positioned between the wall leveling mortar and the coating layer, and plays an auxiliary role of further leveling and forming decorative texture patterns. The putty powder is convenient to package, store and transport, and can be directly constructed by adding water and uniformly stirring on site. The putty powder is prepared by uniformly mixing white cement, inert filler and chemical additive, and the dry powder material is directly added with water and stirred into paste according to the requirement after being transported to a construction site, so that the doctor-blading construction is very convenient. In the decoration of the inner wall of a building, the using amount of the putty powder of the inner wall is increased, and the quality of the putty powder directly influences the decoration effect of the inner wall painting. The traditional putty powder has the defects of low bonding strength, poor water resistance, coating cracking, peeling, falling off, mold growth and the like, most of the putty powder contains glue, formaldehyde and other substances harmful to human bodies exist in the glue, and the environmental protection performance is poor. Along with the social progress, the functional requirements of people on putty powder are gradually improved. How to improve the performance of putty powder on the basis of environmental protection, energy conservation and convenient construction has become the trend of putty development in the future.
Disclosure of Invention
The invention provides interior wall smooth putty powder which comprises the components of desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methyl cellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum modifier, carboxymethyl cellulose, dispersing agent, defoaming agent and mildew inhibitor; the preparation method of the guar gum modifier comprises the following steps:
(1) Dispersing guar gum powder in isopropanol, adding ethanol solution of sodium hydroxide into the solution, stirring the solution after the addition is completed for alkalizing for more than 20min, then carrying out solid-liquid separation, washing the solid phase with ethanol, and drying; adding the dried solid phase into an aqueous solution of 2-chloropropionic acid, continuously stirring for more than 20 minutes in a microwave environment after the addition is finished, then adding sodium hydroxide again, and continuously stirring for more than 20 minutes in the microwave environment after the addition is finished to obtain a guar gum pretreatment mixture;
(2) Uniformly mixing L-malic acid, L-glutamic acid and acetyl chloride in a reaction kettle, heating the mixture to 45+/-2 ℃ in a water bath, preserving heat, adding phosphoric acid into the mixture after the mixture is heated, sealing the reaction kettle after the charging is finished, preserving heat for 10-15 min at 45+/-2 ℃, then preserving heat for more than 30min at 85+/-5 ℃ in the water bath, and air-cooling to normal temperature after the heat preservation is finished; opening the reaction kettle, distilling under reduced pressure to remove acetyl chloride, and then adding ethanol into the reaction kettle;
(3) Adding excessive ethanol into the guar gum pretreatment mixture for precipitation, washing the precipitate with ethanol, and drying; adding the dried solid phase into a reaction kettle, carrying out ice bath to 5+/-2 ℃ after the addition, preserving heat for 1-2 hours, then standing to normal temperature, carrying out solid-liquid separation, washing the solid phase with ethanol, preserving heat for more than 3 hours at the temperature of 70 ℃ for drying, and then carrying out air cooling to normal temperature to obtain the guar gum modified substance.
Further, the preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture after preserving heat, adding tetramethylammonium hydroxide into the mixture in a stirring state, continuing stirring the mixture for more than 4 hours in a heat preserving state of 90+/-2 ℃ after the addition, heating the mixture to 130 ℃ again after the heat preservation is finished, preserving heat for 10-20 min, and then air-cooling to normal temperature;
and step two, adding ethanol into the mixture, heating to 70+/-2 ℃ in an argon atmosphere after the addition, preserving heat, adding epoxy polyether into the mixture after the heat preservation, continuously stirring the mixture for more than 3 hours in the argon atmosphere at the temperature of 70+/-2 ℃ after the addition, and then distilling under reduced pressure to remove the ethanol to obtain the polyether modified silicone oil.
Further, the putty powder comprises the following components in parts by weight: 50 parts of desulfurized gypsum, 20-30 parts of talcum powder, 40-50 parts of heavy calcium carbonate powder, 0.01-0.02 part of hydroxypropyl methyl cellulose, 0.5-0.8 part of chitosan oligosaccharide, 0.03-0.06 part of beta-cyclodextrin, 2-4 parts of polyether modified silicone oil, 1-6 parts of guar gum modifier, 0.1-0.8 part of carboxymethyl cellulose, 1-3 parts of dispersing agent, 0.8-1.2 parts of defoamer and 0.3-0.6 part of mildew preventive.
Further, in the step (1), the guar gum powder is dispersed in isopropanol in an amount ratio of guar gum powder/isopropanol=10 to 15g/100mL; in the ethanol solution of sodium hydroxide, the concentration of the sodium hydroxide is 40-50 g/L, and the volume ratio of the added volume of the ethanol solution of sodium hydroxide to the volume ratio of the isopropanol is the ethanol solution of sodium hydroxide: isopropanol=1:10; in the aqueous solution of the 2-chloropropionic acid, the concentration of the 2-chloropropionic acid is 3-5 g/100mL; the solid-liquid mass ratio of the dried solid phase added into the aqueous solution of 2-chloropropionic acid is solid/liquid=9-14 g/100mL; the added mass of the sodium hydroxide is 0.4 to 0.5 times of the solid phase mass after the drying; the microwave power is 500W.
Further, in the step (2), the mixed molar ratio of the L-malic acid, the L-glutamic acid and the acetyl chloride is L-malic acid: l-glutamic acid: acetyl chloride=5:1 to 2:10; the adding mass of the phosphoric acid is 1% of the acetyl chloride mass; the mass of the ethanol is 10 times of that of the L-malic acid used as the raw material.
Further, in the step (3), the mass of the dried solid phase added into the reaction kettle is 1/8-1/7 of the added mass of the ethanol.
Further, in the first step, the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is the silane coupling agent KH-602: hydroxy silicone oil=3:1-2; the mass ratio of the added tetramethylammonium hydroxide to the silane coupling agent KH-602 is tetramethylammonium hydroxide: silane coupling agent KH-602=0.1 to 0.2:3.
Further, in the second step, ethanol is added to the mixture at a mass ratio of mixture/ethanol=1:20; the addition mass of the epoxy polyether is 1.2-1.4 times of the mass of the mixture.
The invention has the beneficial effects that: the putty powder has good bonding strength and water resistance, improves the service performance of the interior wall putty powder, is not easy to fall off or crack after construction, prolongs the service life, and reduces the maintenance cost of the wall.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1
The putty powder comprises desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methylcellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum modified matters, carboxymethyl cellulose, dispersing agents, defoaming agents and mildew inhibitors; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 20 parts of talcum powder, 40 parts of heavy calcium carbonate powder, 0.01 part of hydroxypropyl methyl cellulose, 0.5 part of chitosan oligosaccharide, 0.03 part of beta-cyclodextrin, 2 parts of polyether modified silicone oil, 1 part of guar gum modified substance, 0.1 part of carboxymethyl cellulose, 1 part of dispersing agent, 0.8 part of defoaming agent and 0.3 part of mildew inhibitor.
The preparation method of the guar gum modifier comprises the following steps:
(1) Guar flour was dispersed in isopropanol in an amount ratio guar flour/isopropanol=10 g/100mL; adding an ethanol solution of sodium hydroxide into the solution, wherein the concentration of the sodium hydroxide in the ethanol solution of sodium hydroxide is 40g/L, and the volume ratio of the added volume of the ethanol solution of sodium hydroxide to the volume ratio of the isopropanol is the ethanol solution of sodium hydroxide: isopropanol=1:10; stirring the solution at a speed of 50r/min after the addition is completed, alkalizing the solution for 20min, then separating solid from liquid, washing the solid phase with ethanol, and drying; adding the dried solid phase into an aqueous solution of 2-chloropropionic acid, wherein the concentration of the 2-chloropropionic acid in the aqueous solution of 2-chloropropionic acid is 3g/100mL; the solid-liquid mass ratio of the dried solid phase added into the aqueous solution of 2-chloropropionic acid is solid/liquid=10 g/100mL; continuously stirring for 20min at a speed of 80r/min in a microwave environment after the addition is finished, then adding sodium hydroxide again, and continuously stirring for 20min in the microwave environment after the addition is finished, wherein the adding mass of the sodium hydroxide is 0.4 time of the mass of the solid phase after the drying; the microwave power is 500W; obtaining a guar gum pretreatment mixture;
(2) Uniformly mixing L-malic acid, L-glutamic acid and acetyl chloride in a reaction kettle, wherein the mixing molar ratio of the L-malic acid to the L-glutamic acid to the acetyl chloride is L-malic acid: l-glutamic acid: acetyl chloride=5:1:10; heating the mixture to 45+/-2 ℃ in a water bath, preserving heat, and adding phosphoric acid into the mixture after the mixture is heated, wherein the adding mass of the phosphoric acid is 1% of the mass of the acetyl chloride; sealing the reaction kettle after the charging is finished, preserving heat for 10min at 45+/-2 ℃, then preserving heat for 30min at 85+/-5 ℃ in a water bath, and air-cooling to normal temperature after the heat preservation is finished; opening the reaction kettle, distilling under reduced pressure to remove acetyl chloride, and then adding ethanol into the reaction kettle, wherein the addition mass of the ethanol is 10 times of the mass of the L-malic acid used by the raw materials;
(3) Adding excessive ethanol into the guar gum pretreatment mixture for precipitation, washing the precipitate with ethanol, and drying; adding the dried solid phase into a reaction kettle, wherein the mass of the dried solid phase added into the reaction kettle is 1/8 of the added mass of the ethanol; and (3) carrying out ice bath to 5+/-2 ℃ after the addition is finished, preserving heat for 1h, then standing to normal temperature, carrying out solid-liquid separation, washing a solid phase by ethanol, preserving heat for 3h at 70 ℃ for drying, and then carrying out air cooling to normal temperature to obtain the guar gum modified substance.
The preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, wherein the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is as follows: hydroxy silicone oil = 3:1; heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture at a speed of 50r/min after the heat preservation, and adding tetramethylammonium hydroxide into the mixture in a stirring state, wherein the mass ratio of the tetramethylammonium hydroxide to the silane coupling agent KH-602 is that the tetramethylammonium hydroxide: silane coupling agent KH-602=0.1:3; continuing stirring the mixture for 4 hours at the temperature of 90+/-2 ℃ after the addition, heating to 130 ℃ again after the heat preservation is finished, preserving the heat for 15 minutes, and then air-cooling to normal temperature;
step two, adding ethanol into the mixture, wherein the mass ratio of the added ethanol is that of the mixture/ethanol=1:20; heating in argon atmosphere to 70+/-2 ℃ after the addition, preserving heat, and adding epoxy polyether into the mixture after the heat preservation, wherein the addition mass of the epoxy polyether is 1.2 times of that of the mixture; and after the addition is finished, continuously stirring the mixture for 3 hours in an argon atmosphere at 70+/-2 ℃ under the heat preservation state, and then distilling under reduced pressure to remove ethanol to obtain the polyether modified silicone oil.
Example 2
The putty powder comprises desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methylcellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum modified matters, carboxymethyl cellulose, dispersing agents, defoaming agents and mildew inhibitors; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 24 parts of talcum powder, 45 parts of heavy calcium carbonate powder, 0.01 part of hydroxypropyl methyl cellulose, 0.6 part of chitosan oligosaccharide, 0.04 part of beta-cyclodextrin, 3 parts of polyether modified silicone oil, 3 parts of guar gum modified substance, 0.4 part of carboxymethyl cellulose, 2 parts of dispersing agent, 1 part of defoaming agent and 0.4 part of mildew preventive.
The preparation method of the guar gum modifier comprises the following steps:
(1) Guar flour was dispersed in isopropanol in an amount ratio guar flour/isopropanol=10 g/100mL; adding an ethanol solution of sodium hydroxide into the solution, wherein the concentration of the sodium hydroxide in the ethanol solution of sodium hydroxide is 40g/L, and the volume ratio of the added volume of the ethanol solution of sodium hydroxide to the volume ratio of the isopropanol is the ethanol solution of sodium hydroxide: isopropanol=1:10; stirring the solution at a speed of 50r/min after the addition is completed, alkalizing the solution for 20min, then separating solid from liquid, washing the solid phase with ethanol, and drying; adding the dried solid phase into an aqueous solution of 2-chloropropionic acid, wherein the concentration of 2-chloropropionic acid in the aqueous solution of 2-chloropropionic acid is 4g/100mL; the solid-liquid mass ratio of the dried solid phase added into the aqueous solution of 2-chloropropionic acid is solid/liquid=10 g/100mL; continuously stirring for 20min at a speed of 80r/min in a microwave environment after the addition is finished, then adding sodium hydroxide again, and continuously stirring for 20min in the microwave environment after the addition is finished, wherein the adding mass of the sodium hydroxide is 0.4 time of the mass of the solid phase after the drying; the microwave power is 500W; obtaining a guar gum pretreatment mixture;
(2) Uniformly mixing L-malic acid, L-glutamic acid and acetyl chloride in a reaction kettle, wherein the mixing molar ratio of the L-malic acid to the L-glutamic acid to the acetyl chloride is L-malic acid: l-glutamic acid: acetyl chloride=5:1:10; heating the mixture to 45+/-2 ℃ in a water bath, preserving heat, and adding phosphoric acid into the mixture after the mixture is heated, wherein the adding mass of the phosphoric acid is 1% of the mass of the acetyl chloride; sealing the reaction kettle after the charging is finished, preserving heat for 10min at 45+/-2 ℃, then preserving heat for 30min at 85+/-5 ℃ in a water bath, and air-cooling to normal temperature after the heat preservation is finished; opening the reaction kettle, distilling under reduced pressure to remove acetyl chloride, and then adding ethanol into the reaction kettle, wherein the addition mass of the ethanol is 10 times of the mass of the L-malic acid used by the raw materials;
(3) Adding excessive ethanol into the guar gum pretreatment mixture for precipitation, washing the precipitate with ethanol, and drying; adding the dried solid phase into a reaction kettle, wherein the mass of the dried solid phase added into the reaction kettle is 1/8 of the added mass of the ethanol; and (3) carrying out ice bath to 5+/-2 ℃ after the addition is finished, preserving heat for 1h, then standing to normal temperature, carrying out solid-liquid separation, washing a solid phase by ethanol, preserving heat for 3h at 70 ℃ for drying, and then carrying out air cooling to normal temperature to obtain the guar gum modified substance.
The preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, wherein the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is as follows: hydroxy silicone oil = 3:1; heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture at a speed of 50r/min after the heat preservation, and adding tetramethylammonium hydroxide into the mixture in a stirring state, wherein the mass ratio of the tetramethylammonium hydroxide to the silane coupling agent KH-602 is that the tetramethylammonium hydroxide: silane coupling agent KH-602=0.1:3; continuing stirring the mixture for 4 hours at the temperature of 90+/-2 ℃ after the addition, heating to 130 ℃ again after the heat preservation is finished, preserving the heat for 15 minutes, and then air-cooling to normal temperature;
step two, adding ethanol into the mixture, wherein the mass ratio of the added ethanol is that of the mixture/ethanol=1:20; heating in argon atmosphere to 70+/-2 ℃ after the addition, preserving heat, and adding epoxy polyether into the mixture after the heat preservation, wherein the addition mass of the epoxy polyether is 1.2 times of that of the mixture; and after the addition is finished, continuously stirring the mixture for 3 hours in an argon atmosphere at 70+/-2 ℃ under the heat preservation state, and then distilling under reduced pressure to remove ethanol to obtain the polyether modified silicone oil.
Example 3
The putty powder comprises desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methylcellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum modified matters, carboxymethyl cellulose, dispersing agents, defoaming agents and mildew inhibitors; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 28 parts of talcum powder, 47 parts of heavy calcium carbonate powder, 0.02 part of hydroxypropyl methyl cellulose, 0.7 part of chitosan oligosaccharide, 0.05 part of beta-cyclodextrin, 3 parts of polyether modified silicone oil, 5 parts of guar gum modified substance, 0.6 part of carboxymethyl cellulose, 2 parts of dispersing agent, 1 part of defoaming agent and 0.5 part of mildew preventive.
The preparation method of the guar gum modifier comprises the following steps:
(1) Guar flour was dispersed in isopropanol in an amount ratio guar flour/isopropanol=10 g/100mL; adding an ethanol solution of sodium hydroxide into the solution, wherein the concentration of the sodium hydroxide in the ethanol solution of sodium hydroxide is 40g/L, and the volume ratio of the added volume of the ethanol solution of sodium hydroxide to the volume ratio of the isopropanol is the ethanol solution of sodium hydroxide: isopropanol=1:10; stirring the solution at a speed of 50r/min after the addition is completed, alkalizing the solution for 20min, then separating solid from liquid, washing the solid phase with ethanol, and drying; adding the dried solid phase into an aqueous solution of 2-chloropropionic acid, wherein the concentration of 2-chloropropionic acid in the aqueous solution of 2-chloropropionic acid is 4g/100mL; the solid-liquid mass ratio of the dried solid phase added into the aqueous solution of 2-chloropropionic acid is solid/liquid=10 g/100mL; continuously stirring for 20min at a speed of 80r/min in a microwave environment after the addition is finished, then adding sodium hydroxide again, and continuously stirring for 20min in the microwave environment after the addition is finished, wherein the adding mass of the sodium hydroxide is 0.4 time of the mass of the solid phase after the drying; the microwave power is 500W; obtaining a guar gum pretreatment mixture;
(2) Uniformly mixing L-malic acid, L-glutamic acid and acetyl chloride in a reaction kettle, wherein the mixing molar ratio of the L-malic acid to the L-glutamic acid to the acetyl chloride is L-malic acid: l-glutamic acid: acetyl chloride=5:2:10; heating the mixture to 45+/-2 ℃ in a water bath, preserving heat, and adding phosphoric acid into the mixture after the mixture is heated, wherein the adding mass of the phosphoric acid is 1% of the mass of the acetyl chloride; sealing the reaction kettle after the charging is finished, preserving heat for 10min at 45+/-2 ℃, then preserving heat for 30min at 85+/-5 ℃ in a water bath, and air-cooling to normal temperature after the heat preservation is finished; opening the reaction kettle, distilling under reduced pressure to remove acetyl chloride, and then adding ethanol into the reaction kettle, wherein the addition mass of the ethanol is 10 times of the mass of the L-malic acid used by the raw materials;
(3) Adding excessive ethanol into the guar gum pretreatment mixture for precipitation, washing the precipitate with ethanol, and drying; adding the dried solid phase into a reaction kettle, wherein the mass of the dried solid phase added into the reaction kettle is 1/8 of the added mass of the ethanol; and (3) carrying out ice bath to 5+/-2 ℃ after the addition is finished, preserving heat for 1h, then standing to normal temperature, carrying out solid-liquid separation, washing a solid phase by ethanol, preserving heat for 3h at 70 ℃ for drying, and then carrying out air cooling to normal temperature to obtain the guar gum modified substance.
The preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, wherein the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is as follows: hydroxy silicone oil = 3:2; heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture at a speed of 50r/min after the heat preservation, and adding tetramethylammonium hydroxide into the mixture in a stirring state, wherein the mass ratio of the tetramethylammonium hydroxide to the silane coupling agent KH-602 is that the tetramethylammonium hydroxide: silane coupling agent KH-602=0.2:3; continuing stirring the mixture for 4 hours at the temperature of 90+/-2 ℃ after the addition, heating to 130 ℃ again after the heat preservation is finished, preserving the heat for 15 minutes, and then air-cooling to normal temperature;
step two, adding ethanol into the mixture, wherein the mass ratio of the added ethanol is that of the mixture/ethanol=1:20; heating in argon atmosphere to 70+/-2 ℃ after the addition, preserving heat, and adding epoxy polyether into the mixture after the heat preservation, wherein the addition mass of the epoxy polyether is 1.2 times of that of the mixture; and after the addition is finished, continuously stirring the mixture for 3 hours in an argon atmosphere at 70+/-2 ℃ under the heat preservation state, and then distilling under reduced pressure to remove ethanol to obtain the polyether modified silicone oil.
Example 4
The putty powder comprises desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methylcellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum modified matters, carboxymethyl cellulose, dispersing agents, defoaming agents and mildew inhibitors; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 30 parts of talcum powder, 50 parts of heavy calcium carbonate powder, 0.02 part of hydroxypropyl methyl cellulose, 0.8 part of chitosan oligosaccharide, 0.06 part of beta-cyclodextrin, 4 parts of polyether modified silicone oil, 6 parts of guar gum modified substance, 0.8 part of carboxymethyl cellulose, 3 parts of dispersing agent, 1.2 parts of defoaming agent and 0.6 part of mildew inhibitor.
The preparation method of the guar gum modifier comprises the following steps:
(1) Guar flour was dispersed in isopropanol in an amount ratio guar flour/isopropanol=10 g/100mL; adding an ethanol solution of sodium hydroxide into the solution, wherein the concentration of the sodium hydroxide in the ethanol solution of sodium hydroxide is 40g/L, and the volume ratio of the added volume of the ethanol solution of sodium hydroxide to the volume ratio of the isopropanol is the ethanol solution of sodium hydroxide: isopropanol=1:10; stirring the solution at a speed of 50r/min after the addition is completed, alkalizing the solution for 20min, then separating solid from liquid, washing the solid phase with ethanol, and drying; adding the dried solid phase into an aqueous solution of 2-chloropropionic acid, wherein the concentration of the 2-chloropropionic acid in the aqueous solution of 2-chloropropionic acid is 5g/100mL; the solid-liquid mass ratio of the dried solid phase added into the aqueous solution of 2-chloropropionic acid is solid/liquid=10 g/100mL; continuously stirring for 20min at a speed of 80r/min in a microwave environment after the addition is finished, then adding sodium hydroxide again, and continuously stirring for 20min in the microwave environment after the addition is finished, wherein the adding mass of the sodium hydroxide is 0.4 time of the mass of the solid phase after the drying; the microwave power is 500W; obtaining a guar gum pretreatment mixture;
(2) Uniformly mixing L-malic acid, L-glutamic acid and acetyl chloride in a reaction kettle, wherein the mixing molar ratio of the L-malic acid to the L-glutamic acid to the acetyl chloride is L-malic acid: l-glutamic acid: acetyl chloride=5:2:10; heating the mixture to 45+/-2 ℃ in a water bath, preserving heat, and adding phosphoric acid into the mixture after the mixture is heated, wherein the adding mass of the phosphoric acid is 1% of the mass of the acetyl chloride; sealing the reaction kettle after the charging is finished, preserving heat for 10min at 45+/-2 ℃, then preserving heat for 30min at 85+/-5 ℃ in a water bath, and air-cooling to normal temperature after the heat preservation is finished; opening the reaction kettle, distilling under reduced pressure to remove acetyl chloride, and then adding ethanol into the reaction kettle, wherein the addition mass of the ethanol is 10 times of the mass of the L-malic acid used by the raw materials;
(3) Adding excessive ethanol into the guar gum pretreatment mixture for precipitation, washing the precipitate with ethanol, and drying; adding the dried solid phase into a reaction kettle, wherein the mass of the dried solid phase added into the reaction kettle is 1/8 of the added mass of the ethanol; and (3) carrying out ice bath to 5+/-2 ℃ after the addition is finished, preserving heat for 1h, then standing to normal temperature, carrying out solid-liquid separation, washing a solid phase by ethanol, preserving heat for 3h at 70 ℃ for drying, and then carrying out air cooling to normal temperature to obtain the guar gum modified substance.
The preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, wherein the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is as follows: hydroxy silicone oil = 3:2; heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture at a speed of 50r/min after the heat preservation, and adding tetramethylammonium hydroxide into the mixture in a stirring state, wherein the mass ratio of the tetramethylammonium hydroxide to the silane coupling agent KH-602 is that the tetramethylammonium hydroxide: silane coupling agent KH-602=0.2:3; continuing stirring the mixture for 4 hours at the temperature of 90+/-2 ℃ after the addition, heating to 130 ℃ again after the heat preservation is finished, preserving the heat for 15 minutes, and then air-cooling to normal temperature;
step two, adding ethanol into the mixture, wherein the mass ratio of the added ethanol is that of the mixture/ethanol=1:20; heating in argon atmosphere to 70+/-2 ℃ after the addition, preserving heat, and adding epoxy polyether into the mixture after the heat preservation, wherein the addition mass of the epoxy polyether is 1.2 times of that of the mixture; and after the addition is finished, continuously stirring the mixture for 3 hours in an argon atmosphere at 70+/-2 ℃ under the heat preservation state, and then distilling under reduced pressure to remove ethanol to obtain the polyether modified silicone oil.
Comparative example 1
The components of the interior wall smooth putty powder used as a contrast comprise desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methyl cellulose, chitosan oligosaccharide, beta-cyclodextrin, guar gum modifier, carboxymethyl cellulose, dispersing agent, defoaming agent and mildew inhibitor; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 28 parts of talcum powder, 47 parts of heavy calcium carbonate powder, 0.02 part of hydroxypropyl methyl cellulose, 0.7 part of chitosan oligosaccharide, 0.05 part of beta-cyclodextrin, 5 parts of guar gum modifier, 0.6 part of carboxymethyl cellulose, 2 parts of dispersing agent, 1 part of defoamer and 0.5 part of mildew inhibitor.
The preparation method of the guar gum modifier comprises the following steps:
(1) Guar flour was dispersed in isopropanol in an amount ratio guar flour/isopropanol=10 g/100mL; adding an ethanol solution of sodium hydroxide into the solution, wherein the concentration of the sodium hydroxide in the ethanol solution of sodium hydroxide is 40g/L, and the volume ratio of the added volume of the ethanol solution of sodium hydroxide to the volume ratio of the isopropanol is the ethanol solution of sodium hydroxide: isopropanol=1:10; stirring the solution at a speed of 50r/min after the addition is completed, alkalizing the solution for 20min, then separating solid from liquid, washing the solid phase with ethanol, and drying; adding the dried solid phase into an aqueous solution of 2-chloropropionic acid, wherein the concentration of 2-chloropropionic acid in the aqueous solution of 2-chloropropionic acid is 4g/100mL; the solid-liquid mass ratio of the dried solid phase added into the aqueous solution of 2-chloropropionic acid is solid/liquid=10 g/100mL; continuously stirring for 20min at a speed of 80r/min in a microwave environment after the addition is finished, then adding sodium hydroxide again, and continuously stirring for 20min in the microwave environment after the addition is finished, wherein the adding mass of the sodium hydroxide is 0.4 time of the mass of the solid phase after the drying; the microwave power is 500W; obtaining a guar gum pretreatment mixture;
(2) Uniformly mixing L-malic acid, L-glutamic acid and acetyl chloride in a reaction kettle, wherein the mixing molar ratio of the L-malic acid to the L-glutamic acid to the acetyl chloride is L-malic acid: l-glutamic acid: acetyl chloride=5:2:10; heating the mixture to 45+/-2 ℃ in a water bath, preserving heat, and adding phosphoric acid into the mixture after the mixture is heated, wherein the adding mass of the phosphoric acid is 1% of the mass of the acetyl chloride; sealing the reaction kettle after the charging is finished, preserving heat for 10min at 45+/-2 ℃, then preserving heat for 30min at 85+/-5 ℃ in a water bath, and air-cooling to normal temperature after the heat preservation is finished; opening the reaction kettle, distilling under reduced pressure to remove acetyl chloride, and then adding ethanol into the reaction kettle, wherein the addition mass of the ethanol is 10 times of the mass of the L-malic acid used by the raw materials;
(3) Adding excessive ethanol into the guar gum pretreatment mixture for precipitation, washing the precipitate with ethanol, and drying; adding the dried solid phase into a reaction kettle, wherein the mass of the dried solid phase added into the reaction kettle is 1/8 of the added mass of the ethanol; and (3) carrying out ice bath to 5+/-2 ℃ after the addition is finished, preserving heat for 1h, then standing to normal temperature, carrying out solid-liquid separation, washing a solid phase by ethanol, preserving heat for 3h at 70 ℃ for drying, and then carrying out air cooling to normal temperature to obtain the guar gum modified substance.
Comparative example 2
The components of the interior wall smooth putty powder used as a contrast comprise desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methyl cellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, carboxymethyl cellulose, a dispersing agent, a defoaming agent and a mildew inhibitor; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 28 parts of talcum powder, 47 parts of heavy calcium carbonate powder, 0.02 part of hydroxypropyl methyl cellulose, 0.7 part of chitosan oligosaccharide, 0.05 part of beta-cyclodextrin, 3 parts of polyether modified silicone oil, 0.6 part of carboxymethyl cellulose, 2 parts of dispersing agent, 1 part of defoamer and 0.5 part of mildew inhibitor.
The preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, wherein the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is as follows: hydroxy silicone oil = 3:2; heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture at a speed of 50r/min after the heat preservation, and adding tetramethylammonium hydroxide into the mixture in a stirring state, wherein the mass ratio of the tetramethylammonium hydroxide to the silane coupling agent KH-602 is that the tetramethylammonium hydroxide: silane coupling agent KH-602=0.2:3; continuing stirring the mixture for 4 hours at the temperature of 90+/-2 ℃ after the addition, heating to 130 ℃ again after the heat preservation is finished, preserving the heat for 15 minutes, and then air-cooling to normal temperature;
step two, adding ethanol into the mixture, wherein the mass ratio of the added ethanol is that of the mixture/ethanol=1:20; heating in argon atmosphere to 70+/-2 ℃ after the addition, preserving heat, and adding epoxy polyether into the mixture after the heat preservation, wherein the addition mass of the epoxy polyether is 1.2 times of that of the mixture; and after the addition is finished, continuously stirring the mixture for 3 hours in an argon atmosphere at 70+/-2 ℃ under the heat preservation state, and then distilling under reduced pressure to remove ethanol to obtain the polyether modified silicone oil.
Comparative example 3
The putty powder comprises desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methylcellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum powder, carboxymethyl cellulose, dispersing agent, defoaming agent and mildew inhibitor; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 28 parts of talcum powder, 47 parts of heavy calcium carbonate powder, 0.02 part of hydroxypropyl methyl cellulose, 0.7 part of chitosan oligosaccharide, 0.05 part of beta-cyclodextrin, 3 parts of polyether modified silicone oil, 5 parts of guar gum powder, 0.6 part of carboxymethyl cellulose, 2 parts of dispersing agent, 1 part of defoaming agent and 0.5 part of mildew preventive.
The preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, wherein the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is as follows: hydroxy silicone oil = 3:2; heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture at a speed of 50r/min after the heat preservation, and adding tetramethylammonium hydroxide into the mixture in a stirring state, wherein the mass ratio of the tetramethylammonium hydroxide to the silane coupling agent KH-602 is that the tetramethylammonium hydroxide: silane coupling agent KH-602=0.2:3; continuing stirring the mixture for 4 hours at the temperature of 90+/-2 ℃ after the addition, heating to 130 ℃ again after the heat preservation is finished, preserving the heat for 15 minutes, and then air-cooling to normal temperature;
step two, adding ethanol into the mixture, wherein the mass ratio of the added ethanol is that of the mixture/ethanol=1:20; heating in argon atmosphere to 70+/-2 ℃ after the addition, preserving heat, and adding epoxy polyether into the mixture after the heat preservation, wherein the addition mass of the epoxy polyether is 1.2 times of that of the mixture; and after the addition is finished, continuously stirring the mixture for 3 hours in an argon atmosphere at 70+/-2 ℃ under the heat preservation state, and then distilling under reduced pressure to remove ethanol to obtain the polyether modified silicone oil.
Example 5
The adhesive strength and alkali resistance of the putty powder of each of the above examples and comparative examples were tested according to the requirements of the standards JG/T298-2010 and GB/T9265-2009, respectively, and the results are shown in Table 1.
TABLE 1
As shown in Table 1, the putty powder provided by the invention has good bonding strength and water resistance, improves the service performance of the interior wall putty powder, prevents the interior wall from falling off and cracking after construction, prolongs the service life, and reduces the maintenance cost of the wall. The comparative example 3 and each comparative example show that the self-made polyether modified silicone oil and guar gum modified substance of the invention are added into the putty powder raw material, so that the bonding performance of the putty powder can be obviously improved, the two substances can play a role in improving the structure of the putty powder, the polymer macromolecules promote the connection among the components of the putty powder, the polymer macromolecules are easy to intertwine, the bonding property and the strength of the putty powder are further improved, the guar gum modified substance is used as a cementing material to obviously optimize the viscosity of the putty powder to a certain extent, the modified guar gum promotes the interaction with other components of the putty powder, and the compactness of the putty powder is improved, so that the putty powder shows better water resistance.
The foregoing detailed description of the embodiments of the present invention will be provided to those skilled in the art, and the detailed description and the examples should not be construed as limiting the invention.
Claims (5)
1. The putty powder for the smooth surface of the inner wall is characterized by comprising the components of desulfurized gypsum, talcum powder, heavy calcium carbonate powder, hydroxypropyl methyl cellulose, chitosan oligosaccharide, beta-cyclodextrin, polyether modified silicone oil, guar gum modifier, carboxymethyl cellulose, dispersing agent, defoaming agent and mildew preventive; the components in parts by weight are as follows: 50 parts of desulfurized gypsum, 20-30 parts of talcum powder, 40-50 parts of heavy calcium carbonate powder, 0.01-0.02 part of hydroxypropyl methyl cellulose, 0.5-0.8 part of chitosan oligosaccharide, 0.03-0.06 part of beta-cyclodextrin, 2-4 parts of polyether modified silicone oil, 1-6 parts of guar gum modifier, 0.1-0.8 part of carboxymethyl cellulose, 1-3 parts of dispersing agent, 0.8-1.2 parts of defoamer and 0.3-0.6 part of mildew preventive; the preparation method of the guar gum modifier comprises the following steps:
(1) Dispersing guar gum powder in isopropanol, adding ethanol solution of sodium hydroxide into the solution, stirring the solution after the addition is completed for alkalizing for more than 20min, then carrying out solid-liquid separation, washing the solid phase with ethanol, and drying; adding the dried solid phase into an aqueous solution of 2-chloropropionic acid, continuously stirring for more than 20 minutes in a microwave environment after the addition is finished, then adding sodium hydroxide again, and continuously stirring for more than 20 minutes in the microwave environment after the addition is finished to obtain a guar gum pretreatment mixture;
(2) Uniformly mixing L-malic acid, L-glutamic acid and acetyl chloride in a reaction kettle, heating the mixture to 45+/-2 ℃ in a water bath, preserving heat, adding phosphoric acid into the mixture after preserving heat, sealing the reaction kettle after feeding, preserving heat for 10-15 min at 45+/-2 ℃, then preserving heat for more than 30min at 85+/-5 ℃ in the water bath, and air-cooling to normal temperature after finishing heat preservation; opening the reaction kettle, distilling under reduced pressure to remove acetyl chloride, and then adding ethanol into the reaction kettle;
(3) Adding excessive ethanol into the guar gum pretreatment mixture for precipitation, washing the precipitate with ethanol, and drying; adding the dried solid phase into a reaction kettle, carrying out ice bath to 5+/-2 ℃ after the addition is completed, preserving heat for 1-2 hours, then standing to normal temperature, carrying out solid-liquid separation, washing the solid phase with ethanol, preserving heat for more than 3 hours at the temperature of 70 ℃ for drying, and then carrying out air cooling to normal temperature to obtain the guar gum modified substance;
the preparation method of the polyether modified silicone oil comprises the following steps:
step one, mixing a silane coupling agent KH-602 and hydroxyl silicone oil to obtain a mixture, heating the mixture to 90+/-2 ℃, preserving heat, stirring the mixture after preserving heat, adding tetramethylammonium hydroxide into the mixture in a stirring state, continuing stirring the mixture for more than 4 hours in a heat preserving state of 90+/-2 ℃ after the addition, heating the mixture to 130 ℃ again after the heat preservation is finished, preserving heat for 10-20 min, and then air-cooling to normal temperature;
and step two, adding ethanol into the mixture, heating to 70+/-2 ℃ in an argon atmosphere after the addition, preserving heat, adding epoxy polyether into the mixture after the heat preservation, continuously stirring the mixture for more than 3 hours in the argon atmosphere at the temperature of 70+/-2 ℃ after the addition, and then distilling under reduced pressure to remove the ethanol to obtain the polyether modified silicone oil.
2. The interior wall finish putty powder according to claim 1, wherein in step (1), the guar gum powder is dispersed in isopropyl alcohol in an amount of guar gum powder/isopropyl alcohol=10 to 15g/100mL; in the ethanol solution of sodium hydroxide, the concentration of the sodium hydroxide is 40-50 g/L, and the volume ratio of the added volume of the ethanol solution of sodium hydroxide to the volume ratio of the isopropanol is the ethanol solution of sodium hydroxide: isopropanol=1:10; in the aqueous solution of the 2-chloropropionic acid, the concentration of the 2-chloropropionic acid is 3-5 g/100mL; the solid solution amount of the dried solid phase added into the aqueous solution of 2-chloropropionic acid is solid/liquid=9-14 g/100mL; the added mass of the sodium hydroxide is 0.4 to 0.5 times of the solid phase mass after the drying; the microwave power is 500W.
3. The interior wall smooth putty powder according to claim 1, wherein in step (2), the mixed molar ratio of L-malic acid, L-glutamic acid and acetyl chloride is L-malic acid: l-glutamic acid: acetyl chloride=5:1 to 2:10; the adding mass of the phosphoric acid is 1% of the acetyl chloride mass; the mass of the ethanol is 10 times of that of the L-malic acid used as the raw material.
4. The interior wall smooth putty powder according to claim 1, wherein in the first step, the mixing mass ratio of the silane coupling agent KH-602 to the hydroxyl silicone oil is the silane coupling agent KH-602: hydroxy silicone oil=3:1-2; the mass ratio of the added tetramethylammonium hydroxide to the silane coupling agent KH-602 is tetramethylammonium hydroxide: silane coupling agent KH-602=0.1 to 0.2:3.
5. The interior wall smooth putty powder according to claim 1, wherein in the second step, ethanol is added to the mixture in a mass ratio of mixture/ethanol=1:20; the mass ratio of the epoxy polyether to the mixture is that the epoxy polyether: mixture = 1.2-1.4: 1.
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| CN116218276A (en) | 2023-06-06 |
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