CN114350189B - Waterproof coating suitable for low-temperature high-humidity environment - Google Patents
Waterproof coating suitable for low-temperature high-humidity environment Download PDFInfo
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- CN114350189B CN114350189B CN202111568096.8A CN202111568096A CN114350189B CN 114350189 B CN114350189 B CN 114350189B CN 202111568096 A CN202111568096 A CN 202111568096A CN 114350189 B CN114350189 B CN 114350189B
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- 238000000576 coating method Methods 0.000 title claims abstract description 72
- 239000011248 coating agent Substances 0.000 title claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000004568 cement Substances 0.000 claims abstract description 36
- 239000000839 emulsion Substances 0.000 claims abstract description 35
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 239000007791 liquid phase Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000007790 solid phase Substances 0.000 claims abstract description 20
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 12
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 11
- 239000004576 sand Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 89
- 239000007789 gas Substances 0.000 claims description 50
- 239000000178 monomer Substances 0.000 claims description 32
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 30
- 239000005977 Ethylene Substances 0.000 claims description 30
- 239000003999 initiator Substances 0.000 claims description 22
- 239000011261 inert gas Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 17
- 238000007599 discharging Methods 0.000 claims description 16
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 15
- 239000003995 emulsifying agent Substances 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000006174 pH buffer Substances 0.000 claims description 11
- 125000004437 phosphorous atom Chemical group 0.000 claims description 9
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 7
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims 1
- 229920006337 unsaturated polyester resin Polymers 0.000 claims 1
- 238000005336 cracking Methods 0.000 abstract description 20
- 238000007720 emulsion polymerization reaction Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 5
- 239000006179 pH buffering agent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- -1 alcohol ester compounds Chemical class 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004078 waterproofing Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical compound [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229940044172 calcium formate Drugs 0.000 description 1
- 235000019255 calcium formate Nutrition 0.000 description 1
- 239000004281 calcium formate Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Paints Or Removers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention provides a waterproof coating suitable for a low-temperature high-humidity environment, which comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 110-130 parts of cement powder, 10-15 parts of fine sand, 10-20 parts of calcium salt powder, 0.1-0.3 part of early strength agent and 0.01-0.03 part of water reducing agent. The liquid phase component comprises: 100 parts of emulsion with the mass concentration of 50-60%, 0.1-0.3 part of defoaming agent, 0.1-0.3 part of film forming agent and 10-30 parts of water. Wherein the emulsion is prepared by vinyl chloride participating in the emulsion polymerization reaction of EVA. The waterproof coating of the invention effectively improves the cracking resistance of the cement-based EVA waterproof coating in low-temperature and high-humidity environment, especially in the waterproof of the internal corner of a building in the low-temperature and high-humidity environment.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a waterproof coating suitable for a low-temperature high-humidity environment.
Background
The cement-based EVA waterproof coating is a very common waterproof coating, can be directly constructed on wet or dry masonry, mortar, concrete, metal, various heat-insulating layers and other waterproof layers, and can be used for buildings or structures such as houses, tunnels, bridges, pools and the like.
However, the existing cement-based EVA waterproof coating often has the problem that cracks appear quickly after the waterproof coating is dried in a low-temperature and high-humidity environment with the temperature of less than or equal to 10 ℃ and the humidity of more than or equal to 80%. Particularly, when the internal corner of a building in a low-temperature high-humidity environment is subjected to waterproof coating, such as a water room of a house, an internal corner of a toilet, the interior of a house separation joint after a rainy day and the like, the cracking problem is more serious, sometimes even if the waterproof coating is not completely dried, the cracking occurs, and the occurrence of the problem seriously influences the waterproof performance of the waterproof coating when the waterproof coating is used in the internal corner of the building in the low-temperature high-humidity environment, particularly the low-temperature high-humidity environment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a waterproof coating suitable for a low-temperature high-humidity environment, which comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 110-130 parts of cement powder, 10-15 parts of fine sand, 10-20 parts of calcium salt powder, 0.1-0.3 part of early strength agent and 0.01-0.03 part of water reducing agent. The liquid phase component comprises: 100 parts of emulsion with the mass concentration of 50-60%, 0.1-0.3 part of defoaming agent, 0.1-0.3 part of film forming agent and 10-30 parts of water.
Further, the preparation method of the emulsion comprises the following steps:
S1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 80-120 parts of water, 0.1-0.3 part of initiator, 3-5 parts of emulsifier, 1-3 parts of polyvinyl alcohol and 0.08-0.12 part of pH buffer agent into a reaction kettle in parts by mass, and fully mixing to obtain a mixed solution.
S2, continuously introducing 40-50 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle, so that the pressure in the reaction kettle is 1.2-2MPa. Simultaneously heating the reaction system to 60-85 ℃.
And S3, after reacting for 6-10 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion.
Further, the step S1 further includes, in parts by mass: 20-25 parts of monomer A, wherein the structural formula of the monomer A is as follows:
wherein R is 1 Is one of C, P and N atoms, R 2 And R 3 The same/different. The R is 2 、R 3 Is C 3 -C 20 Of (a) an alkane. />
Further, said R 2 And R 3 Same, are all C 6 -C 10 Linear alkanes of (1).
Further, said R 1 Is a P atom.
Further, step S1 includes:
s1-1, adding 20-25 parts of monomer A, 30-35 parts of water, 60-65% of initiator, 3-5 parts of emulsifier, 1-3 parts of polyvinyl alcohol and 0.08-0.12 part of pH buffer into a reaction kettle, and fully mixing to obtain a mixed solution.
S1-2, heating the system to 40 +/-2 ℃, maintaining the temperature for 3-5min, adding the balance of water and initiator, and adding 120 parts of vinyl acetate monomer.
And S1-3, maintaining the stirring state in the reaction kettle to obtain the mixed solution. And simultaneously replacing the air in the reaction kettle with inert gas, and performing the step S2 after the replacement is finished.
Further, the mixed gas comprises 10-40% of vinyl chloride and the balance of ethylene in percentage by volume.
Further, the step S2 includes a method of continuously introducing the mixed gas into the reaction kettle: firstly, introducing ethylene gas, and after the introduction amount of the ethylene gas reaches 60-65% of the formula amount, beginning to introduce vinyl chloride gas.
Further, step S2 further includes: and S2-1, after the mixed gas is completely introduced into the reaction kettle, adopting inert gas to continue introducing into the reaction kettle, and maintaining the pressure in the reaction kettle at 2-3MPa.
The invention has the advantages that:
1. the waterproof coating of the invention effectively improves the cracking resistance of the cement-based EVA waterproof coating in low-temperature and high-humidity environment, especially in the waterproof of the internal corner of a building in the low-temperature and high-humidity environment.
2. The invention changes the production process of the existing cement-based EVA waterproof coating less, can realize the production of the novel waterproof coating without replacing large-scale equipment, and obviously reduces the technical improvement cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
The definitions of the radicals and terms described in the specification and claims of the present application, including their definitions as examples, exemplary definitions, preferred definitions, definitions described in the tables, definitions of specific compounds in the examples, etc., may be combined with each other in any combination. The definitions of the groups and the structures of the compounds in such combinations and after the combination are within the scope of the present specification.
The term "C 3 -C 20 "is understood to mean having 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20 carbon atoms," C 6 -C 10 "is understood to mean having 6, 7, 8, 9, 10 carbon atoms," C 10 -C 15 "is understood to mean having 10, 11, 12, 13, 14, 15 carbon atoms," C 6 -C 8 "is understood to mean having 6, 7, 8 carbon atoms.
The cement powder is portland cement, preferably 42.5R, 52.5R and 62.5R cement.
The fine sand of the invention is: 80-120 mesh quartz sand.
The calcium salt powder of the invention can be: 250-300 meshes of heavy calcium carbonate.
The early strength agent of the invention can be: calcium formate.
The water reducing agent provided by the invention can be: a polycarboxylate water reducing agent.
The defoaming agent provided by the invention can be: mineral oil type defoaming agents.
The film forming agent of the invention can be: alcohol ester compounds.
The initiator of the invention can be: potassium persulfate.
The emulsifier of the invention can be: OP-10.
The pH buffering agent of the present invention may be: acetate type pH buffer.
The inert gas in the present invention may be nitrogen.
The following performance test methods are adopted to perform performance tests on the waterproof coatings obtained in the specific examples and the comparative examples:
1. and (3) testing the water impermeability: water pressure of 0.3MPa for 30min.
2. Cracking test: the waterproof coating is smeared at the internal corner of an L-shaped mould prepared by cement, the smearing thickness is 1mm, the L-shaped mould smeared with the waterproof coating is placed in the environments with the temperature of 5 ℃, the temperature of 10 ℃, the humidity of 80% and the humidity of 90% for testing, 5 groups of L-shaped moulds smeared with the same waterproof coating are placed in each environment, after the waterproof coating is completely dried, the L-shaped moulds are continuously placed in the environment for 7 days, and the cracking condition of a coating film is observed.
3. Bonding strength: the test is carried out according to the test method GB/T16777-2008.
Example 1
The waterproof coating suitable for the low-temperature high-humidity environment comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 120 parts of cement powder, 13 parts of fine sand, 15 parts of calcium salt powder, 0.2 part of early strength agent and 0.02 part of water reducing agent. The liquid phase component comprises: 100 parts of emulsion with the mass concentration of 55%, 0.2 part of defoaming agent, 0.2 part of film forming agent and 15 parts of water.
The preparation method of the emulsion comprises the following steps:
s1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 100 parts of water, 0.2 part of initiator, 4 parts of emulsifier, 2 parts of polyvinyl alcohol and 0.1 part of pH buffer agent in parts by mass into a reaction kettle, and fully mixing to obtain a mixed solution.
S2, continuously introducing 45 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle to enable the pressure in the reaction kettle to be 1.5MPa. While heating the reaction system to 75 ℃. The mixed gas comprises 28% of vinyl chloride and the balance of ethylene in volume percentage.
And S3, after reacting for 8 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion.
Example 2
The waterproof coating suitable for the low-temperature high-humidity environment comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 130 parts of cement powder, 15 parts of fine sand, 20 parts of calcium salt powder, 0.3 part of early strength agent and 0.03 part of water reducing agent. The liquid phase component comprises: 100 parts of 60% emulsion, 0.3 part of defoaming agent, 0.3 part of film forming agent and 30 parts of water.
The preparation method of the emulsion comprises the following steps:
s1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 120 parts of water, 0.3 part of initiator, 5 parts of emulsifier, 3 parts of polyvinyl alcohol and 0.12 part of pH buffer agent in parts by mass into a reaction kettle, and fully mixing to obtain a mixed solution.
S2, continuously introducing 50 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle to enable the pressure in the reaction kettle to be 2MPa. While heating the reaction system to 60 ℃. The mixed gas comprises 40% of vinyl chloride and the balance of ethylene by volume percentage.
And S3, after the reaction is carried out for 9 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion.
Example 3
The waterproof coating suitable for the low-temperature high-humidity environment comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 110 parts of cement powder, 10 parts of fine sand, 10 parts of calcium salt powder, 0.1 part of early strength agent and 0.01 part of water reducing agent. The liquid phase component comprises: 100 parts of 50% emulsion, 0.1 part of defoaming agent, 0.1 part of film forming agent and 10 parts of water.
The preparation method of the emulsion comprises the following steps:
s1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 80 parts of water, 0.1 part of initiator, 3 parts of emulsifier, 1 part of polyvinyl alcohol and 0.08 part of pH buffering agent in parts by mass into a reaction kettle, and fully mixing to obtain a mixed solution.
S2, continuously introducing 40-50 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle to enable the pressure in the reaction kettle to be 1.2MPa. While heating the reaction system to 85 ℃. The mixed gas comprises 10% of vinyl chloride and the balance of ethylene in percentage by volume.
And S3, after the reaction is carried out for 7 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion.
Example 4
The waterproof coating suitable for the low-temperature high-humidity environment comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 120 parts of cement powder, 13 parts of fine sand, 15 parts of calcium salt powder, 0.2 part of early strength agent and 0.02 part of water reducing agent. The liquid phase component comprises: 100 parts of emulsion with the mass concentration of 55%, 0.2 part of defoaming agent, 0.2 part of film forming agent and 15 parts of water.
The preparation method of the emulsion comprises the following steps:
s1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 22 parts of monomer A, 100 parts of water, 0.2 part of initiator, 4 parts of emulsifier, 2 parts of polyvinyl alcohol and 0.1 part of pH buffer in parts by mass into a reaction kettle, and fully mixing to obtain a mixed solution. The structural formula of the monomer A is as follows:
S2, continuously introducing 45 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle to enable the pressure in the reaction kettle to be 1.5MPa. While heating the reaction system to 63 ℃. The mixed gas comprises 28% of vinyl chloride and the balance of ethylene in volume percentage.
And S3, after reacting for 10 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion.
Example 5
The waterproof coating suitable for the low-temperature high-humidity environment comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 120 parts of cement powder, 13 parts of fine sand, 15 parts of calcium salt powder, 0.2 part of early strength agent and 0.02 part of water reducing agent. The liquid phase component comprises: 100 parts of emulsion with the mass concentration of 55%, 0.2 part of defoaming agent, 0.2 part of film forming agent and 15 parts of water.
The preparation method of the emulsion comprises the following steps:
s1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 25 parts of monomer A, 100 parts of water, 0.2 part of initiator, 4 parts of emulsifier, 2 parts of polyvinyl alcohol and 0.1 part of pH buffering agent in parts by mass into a reaction kettle, and fully mixing to obtain a mixed solution. The structural formula of the monomer A is as follows:
Wherein R is 1 Is a C atom, R 2 And R 3 Different. The R is 2 Is C 3 Alkane of (A), R 3 Is C 20 Of (a) an alkane.
S2, continuously introducing 45 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle to enable the pressure in the reaction kettle to be 1.5MPa. While heating the reaction system to 63 ℃. The mixed gas comprises 28% of vinyl chloride and the balance of ethylene in volume percentage.
And S3, after reacting for 10 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion.
Example 6
The waterproof coating suitable for the low-temperature high-humidity environment comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 120 parts of cement powder, 13 parts of fine sand, 15 parts of calcium salt powder, 0.2 part of early strength agent and 0.02 part of water reducing agent. The liquid phase component comprises: 100 parts of emulsion with the mass concentration of 55%, 0.2 part of defoaming agent, 0.2 part of film forming agent and 15 parts of water.
The preparation method of the emulsion comprises the following steps:
s1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 20 parts of monomer A, 100 parts of water, 0.2 part of initiator, 4 parts of emulsifier, 2 parts of polyvinyl alcohol and 0.1 part of pH buffering agent in parts by mass into a reaction kettle, and fully mixing to obtain a mixed solution. The structural formula of the monomer A is as follows:
S2, continuously introducing 45 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle to enable the pressure in the reaction kettle to be 1.5MPa. While heating the reaction system to 63 ℃. The mixed gas comprises 28% of vinyl chloride and the balance of ethylene in volume percentage.
And S3, after reacting for 10 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion.
Comparative example 1
The waterproof coating comprises a solid-phase component and a liquid-phase component, wherein the solid-phase component comprises the following components in parts by mass: 120 parts of cement powder, 13 parts of fine sand, 15 parts of calcium salt powder, 0.2 part of early strength agent and 0.02 part of water reducing agent. The liquid phase component comprises: 100 parts of emulsion with the mass concentration of 55%, 0.2 part of defoaming agent, 0.2 part of film forming agent and 15 parts of water. The emulsion is EVA emulsion.
Comparative example 2
The waterproof coating is prepared and compatible by adopting the method of example 1, and the differences are as follows: the mixed gas comprises 50% of vinyl chloride and the balance of ethylene in volume percentage.
Comparative example 3
The waterproof coating is prepared and compatible by adopting the method of example 1, and the differences are as follows: the mixed gas comprises 5% of vinyl chloride and the balance of ethylene in volume percentage.
Comparative example 4
The waterproof coating is prepared and compatible by the method of example 4, with the difference that: the mixed gas comprises 50% of vinyl chloride and the balance of ethylene in volume percentage.
Comparative example 5
The waterproof coating is prepared and compatible by the method of example 4, with the difference that: the mixed gas comprises 5% of vinyl chloride and the balance of ethylene in volume percentage.
Comparative example 6
The waterproof coating is prepared and compatible by the method of example 4, with the difference that: the amount of the monomer A added was changed to 30 parts.
Comparative example 7
The waterproof coating is prepared and compatible by the method of example 4, with the difference that: the amount of the monomer A added was changed to 15 parts.
Examples 1-7 the results of the performance tests are given in the following table:
as shown in comparative example 1, when the existing cement-based EVA waterproof coating is used for smearing water on the internal corner of a building with low temperature and high humidity, although a test sample is subjected to a water impermeability test to reach the water impermeability level of 0.3MPa for 30min, in the environment of simulating the internal corner of the building with low temperature and high humidity, the coating has a high probability of generating a cracking phenomenon in 7 days actually, which is shown as the occurrence of cracks on the surface of the coating. Once the waterproof coating cracks, the waterproof performance of the waterproof coating is basically mostly lost.
The emulsion obtained by using a certain amount of VCM to participate in the copolymerization reaction of EVA is used as the emulsion part of the cement-based EVA waterproof coating, so that the cracking phenomenon of the cement-based EVA waterproof coating when the cement-based EVA waterproof coating is coated on the internal corner of a building with low temperature and high humidity for waterproofing can be obviously improved. However, as shown in comparative examples 2 to 5, the cracking resistance of the cement-based EVA waterproof coating material was rather significantly reduced when VCM was used in an amount exceeding a certain amount (e.g., 50% by volume). And insufficient VCM (such as 5% of volume fraction) is adopted, the cracking resistance of the cement-based EVA waterproof coating is close to that of the common cement-based EVA waterproof coating, and the cement-based EVA waterproof coating cannot have a due modification effect. Therefore, only a proper amount of VCM participates in the copolymerization of EVA, the cracking resistance of the cement-based EVA waterproof coating can be obviously improved, and especially the cracking resistance when the cement-based EVA waterproof coating is used in the internal corner environment of a building with low temperature and high humidity.
As can be seen by comparing examples 4 to 7 with examples 1 to 3,the modified EVA emulsion prepared by adding the monomer is used as the emulsion part of the cement-based EVA waterproof coating, so that the bonding strength of the cement-based EVA waterproof coating is improved, and the anti-cracking performance of the cement-based EVA waterproof coating in the low-temperature and high-humidity building internal corner environment is improved It appeared that crazing and cracking hardly occurred any more. However, as shown in comparative examples 6 and 7, the monomer A in an amount exceeding a certain amount does not continue to exert the effect of improving the crack resistance of the cement-based EVA waterproofing paint, while the monomer A in an insufficient amount causes the occurrence of the crazing phenomenon. The crazes are likely to be converted into cracks in the process of later continuous use. />
In order to further study the improvement of the cracking resistance of each atom in the monomer A to the cement-based EVA waterproof coating, the applicant selects R of the monomer A respectively by using the preparation method of example 4 as an expansion test 1 Cracking experiments were performed on 4 groups of coatings with C, P, N atoms, with selected experimental conditions of 5 deg.C, 90% humidity, and 50 samples per group. The experimental results are as follows: r 1 When P atoms were used, no silver streaks were generated in all 50 groups of samples. R 1 In the case of C atoms, 14 groups of samples produced 1-2 unequal silver streaks within 7 days. R 1 For N atoms, 6 groups of samples produced 1-2 unequal silver streaks within 7 days. It can be seen that although R in monomer A is 1 When the component is one of C, P and N, the cracking resistance of the cement-based EVA waterproof coating in the low-temperature and high-humidity building internal corner environment can be improved. But when R in the monomer A is 1 When the P atom is contained, the modified cement-based EVA waterproof coating has the cracking resistance effect in the low-temperature and high-humidity building internal corner environment which is obviously better than that of the other 3 atoms.
Example 8
Based on the waterproof coating material suitable for low-temperature and high-humidity environment described in examples 4 to 7, step S1 includes:
s1-1, adding 22 parts of monomer A, 33 parts of water, 62% of initiator, 4 parts of emulsifier, 2 parts of polyvinyl alcohol and 0.1 part of pH buffer agent into a reaction kettle, and fully mixing to obtain a mixed solution.
S1-2, heating the system to 40 +/-2 ℃, maintaining for 4min, adding the balance of water and initiator, and adding 120 parts of vinyl acetate monomer.
And S1-3, maintaining the stirring state in the reaction kettle to obtain the mixed solution. And simultaneously replacing the air in the reaction kettle with inert gas, and performing the step S2 after the replacement is finished.
Example 9
Based on the waterproof coating material suitable for low-temperature and high-humidity environment described in examples 4 to 7, step S1 includes:
s1-1, adding 25 parts of monomer A, 35 parts of water, 65% of initiator, 5 parts of emulsifier, 3 parts of polyvinyl alcohol and 0.12 part of pH buffer agent into a reaction kettle, and fully mixing to obtain a mixed solution.
S1-2, heating the system to 40 +/-2 ℃, maintaining for 5min, adding the balance of water and initiator, and adding 120 parts of vinyl acetate monomer.
And S1-3, maintaining the stirring state in the reaction kettle to obtain the mixed solution. And simultaneously replacing the air in the reaction kettle with inert gas, and performing the step S2 after the replacement is finished.
Example 10
Based on the waterproof coating material suitable for low-temperature and high-humidity environment described in examples 4 to 7, step S1 includes:
s1-1, adding 20 parts of monomer A, 30 parts of water, 60% of initiator, 3 parts of emulsifier, 1 part of polyvinyl alcohol and 0.08 part of pH buffer agent into a reaction kettle, and fully mixing to obtain a mixed solution.
S1-2, heating the system to 40 +/-2 ℃, maintaining for 3min, adding the balance of water and initiator, and adding 120 parts of vinyl acetate monomer.
And S1-3, maintaining the stirring state in the reaction kettle to obtain the mixed solution. And simultaneously replacing the air in the reaction kettle with inert gas, and performing the step S2 after the replacement is finished.
In examples 4 to 7, since the monomer A was directly mixed with the compounding amounts of the vinyl acetate monomer, water, initiator and other auxiliary agents, the reaction time required in step S3 was 10 hours. By adopting the method of the embodiment 8-10, the monomer A is firstly mixed with a certain amount of water and initiator, and the rest of the auxiliary agent according to the formula amount, then the temperature is kept at 40 +/-2 ℃ for 3-5min, and then the rest of the water, the initiator and the vinyl acetate monomer according to the formula amount are added. Although one step is additionally added in the process and the temperature needs to be additionally kept for 3-5min, the reaction time needed in the step S3 is reduced to 9 hours, and the overall production efficiency is obviously improved.
Example 11
Based on the waterproof coating suitable for the low-temperature and high-humidity environment described in examples 4 to 7, the method for continuously introducing the mixed gas into the reaction kettle in step S2 includes: the ethylene gas is firstly introduced, and the introduction of the vinyl chloride gas is started after the introduction amount of the ethylene gas reaches 60 to 65 percent, preferably 63 percent of the formula amount.
During the enlarged cracking experiment, the method of adding the mixed gas of vinyl chloride and ethylene in one time as described in example 4 is adopted, and the ratio of the monomer A: r 1 When P atoms were used, no silver streaks were generated in all 50 groups of samples. R 1 In the case of C atoms, 14 groups of samples produced 1-2 unequal silver streaks within 7 days. R is 1 For N atoms, 6 groups of samples produced 1-2 unequal silver streaks within 7 days. However, as a result of controlling the supply of ethylene gas and vinyl chloride gas by the method described in example 11, the ratio of monomer A: r is 1 When P and N atoms were used, silver streaks were not generated in all 50 groups of samples. R 1 For the C atom, 1 silver streak was generated in 7 days for 2 groups of samples. And R is 1 When the monomer A is C atom, the alkyl group graft modification monomer of styrene is adopted as the monomer A, compared with heteroatom aryl, the difficulty in obtaining phenyl and the preparation cost are obviously reduced, and the method of the embodiment 11 is adopted to control the introduction mode of ethylene gas and chloroethylene gas, so that the R can be obviously improved 1 When the carbon atom is C, the cracking resistance of the cement-based EVA waterproof coating in the low-temperature and high-humidity building internal corner environment is improved, so that the preparation cost of the product is obviously reduced on the basis of meeting the use requirement.
Example 12
Based on the waterproof coating material suitable for low-temperature and high-humidity environment described in examples 4 to 7, step S2 further includes: and S2-1, after the mixed gas is completely introduced into the reaction kettle, adopting inert gas to continue introducing into the reaction kettle, and maintaining the pressure in the reaction kettle at 2-3MPa.
In examples 4 to 7, after the mixed gas of vinyl chloride and ethylene was introduced, the inert gas was not introduced any more, and as the reaction proceeded, the mixed gas in the reaction vessel decreased and the pressure decreased, so that the reaction in step S3 took 10 hours to obtain the emulsion product. By maintaining the pressure in the reaction vessel by adding the inert gas in the method described in example 12, the monomer mixture can be forced to participate in the polymerization reaction, thereby significantly reducing the reaction time required for step S3.
The reaction time of step S3 can be reduced to about 7 hours by using the pressure control method of example 12 alone without changing other conditions. By combining the methods of examples 8-10, the overall reaction time can be reduced to about 6 hours, and the preparation efficiency of the emulsion is remarkably improved.
It is to be noted and understood that various modifications and improvements can be made to the invention described in detail above without departing from the spirit and scope of the invention as claimed. Accordingly, the scope of the claimed subject matter is not limited by any of the specific exemplary teachings provided.
Claims (7)
1. The waterproof coating suitable for the low-temperature high-humidity environment comprises a solid-phase component and a liquid-phase component, and is characterized in that the solid-phase component comprises the following components in parts by mass: 110-130 parts of cement powder, 10-15 parts of fine sand, 10-20 parts of calcium salt powder, 0.1-0.3 part of early strength agent and 0.01-0.03 part of water reducing agent; the liquid phase component comprises: 100 parts of emulsion with the mass concentration of 50-60%, 0.1-0.3 part of defoaming agent, 0.1-0.3 part of film forming agent and 10-30 parts of water;
the preparation method of the emulsion comprises the following steps:
s1, under the protection of inert gas, adding 120 parts of vinyl acetate monomer, 80-120 parts of water, 0.1-0.3 part of initiator, 3-5 parts of emulsifier, 1-3 parts of polyvinyl alcohol and 0.08-0.12 part of pH buffer into a reaction kettle in parts by mass, and fully mixing to obtain a mixed solution;
s2, continuously introducing 40-50 parts of mixed gas of vinyl chloride and ethylene into the reaction kettle, so that the pressure in the reaction kettle is 1.2-2MPa; simultaneously heating the reaction system to 60-85 ℃;
S3, after reacting for 6-10 hours, discharging gas in the reaction kettle, and discharging a liquid phase part in the reaction kettle after the pressure in the reaction kettle is relieved to normal pressure to obtain the emulsion;
the step S1 further comprises the following steps in parts by mass: 20-25 parts of monomer A, wherein the structural formula of the monomer A is as follows:
2. The waterproof coating material suitable for low-temperature and high-humidity environment according to claim 1, wherein R is 2 And R 3 Same, are all C 6 -C 10 Linear alkanes of (1).
3. The waterproof coating material for a low-temperature high-humidity environment according to claim 1, wherein R is an unsaturated polyester resin 1 Is a P atom.
4. The waterproof coating material suitable for a low-temperature and high-humidity environment according to claim 1, wherein the step S1 comprises:
s1-1, adding 20-25 parts of monomer A, 30-35 parts of water, 60-65% of initiator, 3-5 parts of emulsifier, 1-3 parts of polyvinyl alcohol and 0.08-0.12 part of pH buffer agent into a reaction kettle in parts by mass, and fully mixing to obtain a mixed solution;
s1-2, heating the system to 40 +/-2 ℃, maintaining the temperature for 3-5min, adding the balance of water and initiator, and adding 120 parts of vinyl acetate monomer;
S1-3, maintaining the stirring state in the reaction kettle to obtain the mixed liquid; and simultaneously replacing the air in the reaction kettle with inert gas, and performing the step S2 after the replacement is finished.
5. The waterproof coating material suitable for a low-temperature and high-humidity environment according to claim 1, wherein the mixed gas comprises 10 to 40% by volume of vinyl chloride and the balance of ethylene.
6. The waterproof coating material suitable for the low-temperature high-humidity environment according to claim 1, wherein the method of continuously introducing the mixed gas into the reaction kettle in the step S2 comprises: firstly, introducing ethylene gas, and after the introduction amount of the ethylene gas reaches 60-65% of the formula amount, beginning to introduce vinyl chloride gas.
7. The waterproof coating material suitable for a low-temperature and high-humidity environment according to claim 1, wherein the step S2 further comprises: and S2-1, after the mixed gas is completely introduced into the reaction kettle, continuously introducing inert gas into the reaction kettle, and maintaining the pressure in the reaction kettle to be 2-3MPa.
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DE2007793A1 (en) * | 1970-02-20 | 1971-08-26 | Bayer Ag | Process for the continuous Her position of copolymer dispersions |
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DE3571998D1 (en) * | 1984-01-20 | 1989-09-07 | Air Prod & Chem | Metal container coating compostions comprising stable emulsions of water resistant vinyl chloride-ethylene copolymers |
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