CN107459655B - Environment-friendly low-VOC interface treating agent and preparation method thereof - Google Patents
Environment-friendly low-VOC interface treating agent and preparation method thereof Download PDFInfo
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- CN107459655B CN107459655B CN201710708114.5A CN201710708114A CN107459655B CN 107459655 B CN107459655 B CN 107459655B CN 201710708114 A CN201710708114 A CN 201710708114A CN 107459655 B CN107459655 B CN 107459655B
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- 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
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C08G81/024—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/0206—Polyalkylene(poly)amines
- C08G73/0213—Preparatory process
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/02—Polyamines
Abstract
The invention provides an environment-friendly low-VOC interface treating agent which is prepared by carrying out polymerization reaction on magnesium trisilicate grafted with polyethyleneimine and polyvinyl acetate emulsion. The magnesium trisilicate is hydrous magnesium silicate, can be produced from industrial raw materials, has a developed pore structure and a large specific surface area, and has good adsorption performance, ion exchange performance and molecular sieve functions, so that the magnesium trisilicate can be used for long-acting absorption of acidic substances generated by degradation of polyvinyl acetate through chemical reaction by utilizing the characteristics of the magnesium trisilicate and for long-acting adsorption and inhibition of emission of organic small molecular impurities through physical action. Meanwhile, non-volatile macromolecular polyethyleneimine with multi-active functional group amino is utilized to rapidly absorb residual vinyl monomers, aldehyde impurities and acidic degradation byproducts through chemical reactions such as Michael addition, amino addition and the like. The prepared interface treating agent has lower VOC and excellent viscosity.
Description
Technical Field
The invention relates to the technical field of interface agents, in particular to an environment-friendly low-VOC interface treating agent and a preparation method thereof.
Background
The concrete interface treating agent is also called concrete interface adhesive, interface treating agent and the like, and is called interface agent for short. The surface treatment material is a functional adhesive and is applied to enhancing the surface performance of concrete. Engineering practice proves that the concrete interface treating agent is an effective technical measure for preventing the plastering layer and the base wall from cracking, separating and peeling. The interface treating agent is used and developed quickly in recent years, and in order to standardize the product performance and ensure the engineering quality, China released the building material industry standard JC 907-. The interfacial agent is divided into two categories according to the composition, namely a dry powder interfacial agent and a liquid interfacial agent. The dry powder interface agent is a dry powder product consisting of inorganic cementing materials such as cement, filler, polymer rubber powder and related additives, and needs to be mixed with water or other liquid mixtures when in use. The liquid interface agent is a product containing polymer dispersion liquid, can be directly coated and used at an interface when in use, and can also be matched with inorganic cementing materials such as cement and the like and water and the like according to a proportion for use. For building interior decoration, the smoother and lower adhesive force of the wall surface, the interface treating agent is coated, one part of the interface agent permeates into the base layer and is embedded into the base layer like an anchor to form a hook system, the adhesive force is improved, and the other part of the interface agent forms an unsmooth and rough air-permeable adhesive film on the surface of the base layer. The adhesive film base layer absorbs part of water to be softened in the plastering or putty-scraping process, so that the bonding of an interface is facilitated, and the effect of improving the interface adhesion of the base layer is achieved. The interface agent can also be used for 'roughening', wherein one part of the interface agent and the cement slurry permeate into the base layer and are embedded into the base layer like an anchor, and the other part of the interface agent and the cement slurry form uneven pointed cement slurry burrs on the base layer of the wall surface. For example, tiles are easy to fall off when being pasted on a smooth wall surface, and the contact area and the base layer adhesive force can be greatly improved by using the interface treating agent.
Most of the interface treating agents disclosed at present are dry powder type interface agents, and less liquid type interface agents are used. Patent CN102643059 discloses a concrete inorganic interface cementation treatment agent, which consists of portland cement, a water reducing agent, a siliceous material, heavy calcium carbonate powder, a water retaining agent, redispersible latex powder, thickening agent modified bentonite and a mineral admixture and is used for repairing and bonding concrete, bonding the surface of a large-volume concrete construction warehouse, and the like. Patent CN 103755223 discloses a concrete interface treating agent composed of epoxy resin, acrylic acid, calcium formate, quartz sand and heavy calcium carbonate powder. Patent CN 104261764 discloses a shrinkage-reducing concrete interface treating agent, which consists of a shrinkage-reducing agent, ethylene-vinyl acetate copolymer emulsion, hydroxypropyl methyl cellulose ether, a film-forming auxiliary agent, a defoaming agent, a polycarboxylic acid high-efficiency water reducing agent, ordinary portland cement, silica fume and water, and is used for treating the interfaces between concrete poured successively at the construction joint of a concrete structure or the interfaces between new and old concrete during structural repair.
The liquid interfacial agent is used for building interior decoration, but volatile small molecular organic compounds are inevitably contained in the components such as emulsion, auxiliary agents and the like used in the interfacial agent, so that the total content of Volatile Organic Compounds (VOCs) in the product is higher, the environmental protection requirements of people are difficult to meet, the increasingly severe environmental protection standards cannot be met, the reduction of the content of the VOCs is the target of current technical development, and the interfacial agent is also a main problem which needs to be solved urgently in scientific research and production in recent years. The product specified by the Chinese environmental protection standard HJ 2541-2016 does not contain phthalate plasticizers, alkylphenol polyoxyethylene ether emulsifiers, isothiazolinone preservatives and the like, and the total volatile organic matter content in the water-based building adhesive is specified to be less than or equal to 40g/L, and the execution of the requirements makes the environmental label product in China more approximate to the ecological label requirements of national regions such as northern Europe, Canada, Australia and the like, so that the traditional polymer emulsion, liquid interface agents, adhesives and the like are challenged, and new technologies are urgently needed to meet the requirements of volatile organic matter content and environmental protection.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide an environment-friendly low-VOC interface treating agent and a preparation method thereof, which has a low VOC content.
The environment-friendly low-VOC interface treating agent provided by the invention is prepared by carrying out polymerization reaction on magnesium trisilicate grafted with polyethyleneimine and polyvinyl acetate emulsion.
The mass ratio of the magnesium trisilicate grafted with polyethyleneimine to the polyvinyl acetate emulsion is preferably (0.1-1): (75.65-129.25).
Preferably, the magnesium trisilicate grafted with polyethyleneimine is obtained by reacting polyethyleneimine and magnesium trisilicate under the action of a silane coupling agent.
Specifically, the magnesium trisilicate grafted with polyethyleneimine is prepared according to the following method:
A) activating magnesium trisilicate by adopting a silane coupling agent under an acidic condition;
B) reacting the activated magnesium trisilicate obtained in the step A) with polyethyleneimine to obtain the polyethyleneimine grafted magnesium trisilicate.
The silane coupling agent is preferably 3- (methacryloyloxy) propyltrimethoxysilane.
According to the invention, the hydrolysis grafting reaction of 3- (methacryloyloxy) propyl trimethoxy silane and the Michael addition reaction of double bonds and amino are utilized to graft polyethyleneimine to magnesium trisilicate to form an organic-inorganic hybrid, and the hybrid is polymerized with polyvinyl acetate emulsion, so that the VOC removing effect is achieved, and the magnesium trisilicate can be uniformly dispersed and suspended in an emulsion system without sedimentation, thereby improving the viscosity of the emulsion.
In step a) above, the activated solvent is preferably ethanol.
In the above step B), the solvent for the reaction is preferably tetrahydrofuran.
The interface treating agent provided by the invention is prepared from vinyl acetate, polyvinyl alcohol, ammonium persulfate, an emulsifier, sodium bicarbonate, water, a plasticizer, a preservative and magnesium trisilicate grafted with polyethyleneimine by emulsion polymerization, physical mixing and other modes, wherein the added magnesium trisilicate grafted with polyethyleneimine can effectively reduce the VOC content and also has a thickening effect on the interface agent, so that the system meets the environmental protection requirement.
The invention provides a preparation method of the environment-friendly low-VOC interface treating agent, which comprises the following steps:
dissolving polyvinyl alcohol in water, adding an emulsifier, ammonium persulfate and vinyl acetate to perform a first polymerization reaction, adding sodium bicarbonate and magnesium trisilicate grafted with polyethyleneimine to perform a second cross-linking polymerization reaction, and finally adding a plasticizer and a preservative to obtain the interface treating agent.
Preferably, the mass ratio of the magnesium trisilicate, vinyl acetate, polyvinyl alcohol, ammonium persulfate, emulsifier, sodium bicarbonate, water, plasticizer and preservative of the grafted polyethyleneimine is (0.1-1): (10-30): (3-4): (0.2-0.3): (0.2-0.4): (0.15-0.25): (60-90): (2-4): (0.1-0.3).
The emulsifier is preferably alkoxy polyethylene hydroxyl ethanol; the plasticizer is preferably dipropylene glycol dibenzoate; the preservative is preferably didecyl dimethyl ammonium chloride.
Preferably, the temperature of the first polymerization reaction is 70 ℃, and the reaction time is 3-6 h.
Preferably, the temperature of the second cross-linking polymerization reaction is 50 ℃, and the reaction time is 1-2 h.
Compared with the prior art, the environment-friendly low-VOC interface treating agent is prepared by carrying out polymerization reaction on magnesium trisilicate grafted with polyethyleneimine and polyvinyl acetate emulsion, and effectively solves the problems of high volatility and environmental pollution of the traditional interface treating agent.
The magnesium trisilicate is hydrous magnesium silicate, can be produced from industrial raw materials, has a developed pore structure and a large specific surface area, and has good adsorption performance, ion exchange performance and molecular sieve functions, so that the magnesium trisilicate can be used for long-acting absorption of acidic substances generated by degradation of polyvinyl acetate through chemical reaction by utilizing the characteristics of the magnesium trisilicate and for long-acting adsorption and inhibition of emission of organic small molecular impurities through physical action.
Meanwhile, non-volatile macromolecular polyethyleneimine with multi-active functional group amino is utilized to rapidly absorb residual vinyl monomers, aldehyde impurities and acidic degradation byproducts through chemical reactions such as Michael addition, amino addition and the like.
Third, the liquid interface processing agent usually has a low concentration when used, and needs a certain viscosity when directly coated or used for cement and wool making, but the viscosity of the general emulsion is not enough after being diluted, and the viscosity must be increased with the help of a thickening and tackifying structure, and traditionally, aldehydes substances, such as formaldehyde and other toxic and harmful compounds, are used to crosslink polyvinyl alcohol to obtain polyvinyl formal. The system of the invention is different from the traditional system, utilizes an organic-inorganic hybrid, not only has the function of reducing volatility, but also can improve thixotropy, has the functions of thickening and improving adhesion, further meets the service performance of the interface agent, and does not need thickening and tackifying structural assistance.
Fourthly, in the interface treating agent provided by the invention, the compatibility of the environment-friendly auxiliary agent and an interface treating agent system is good, the types of ionic systems can be fused with each other, the emulsion is stable, the integral comprehensive performance and functions can be met, and the requirements of environment-friendly standards can be met.
Detailed Description
In order to further illustrate the present invention, the following will describe the environmental-friendly low-VOC interface treating agent and the preparation method thereof in detail with reference to the examples.
Comparative example 1
Adding 8kg of water into a dissolving kettle, adding 0.3kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.41kg of vinyl acetate into the polymerization kettle, dropwise reacting for 6 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, reacting for 2 hours, adding 0.2kg of plasticizer and 10g of preservative, cooling to room temperature, and discharging to obtain an interface treating agent contrast sample, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The total volatile organic content was tested by gas chromatography in standard appendix F of GB 18583-2008 "Limit of hazardous substances in adhesive for interior decorative materials", and the TVOC content of the comparative sample of interface treating agent was 47 g/L. The viscosity was measured by a rotary viscometer and found to be 200 mPas.
Example 1
Preparation of polyethyleneimine grafted magnesium trisilicate:
dispersing 10g of magnesium trisilicate in 500 g of ethanol, adding 0.1 g of hydrochloric acid and 50g of 3- (methacryloyloxy) propyl trimethoxy silane, stirring at 50 ℃ for reaction for 12 hours, filtering, dispersing solid powder in 500 g of tetrahydrofuran, adding 50g of polyethyleneimine, stirring at 50 ℃ for reaction for 24 hours, filtering, putting the solid powder in a vacuum drying oven, and drying at 60 ℃ for 24 hours to finally obtain the magnesium trisilicate grafted with the polyethyleneimine.
Example 2
Preparing a concrete interface treating agent: firstly, adding 8kg of water into a dissolving kettle, adding 0.3kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.41kg of vinyl acetate into the polymerization kettle, dropwise reacting for 6 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 10g of magnesium trisilicate grafted with polyethyleneimine, reacting for 2 hours, adding 0.2kg of plasticizer and 10g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting the gas chromatography in standard appendix F of GB 18583 + 2008 'Limited harmful substance in adhesive for interior decoration Material', the TVOC content of an interface treating agent is 37g/L, compared with a sample of a comparative example, the TVOC content is reduced by 21.3%, the compatibility among components is good, the viscosity is 2100mPa & s after being tested by a rotary viscometer, the proper consistency is ensured, no settlement is generated, and the requirement of the Chinese environmental protection standard HJ 2541 + 2016 'adhesive for environmental Mark product technical requirement' is met.
Example 3
Preparing a concrete interface treating agent: firstly, adding 8kg of water into a dissolving kettle, adding 0.3kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.41kg of vinyl acetate into the polymerization kettle, dropwise reacting for 6 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 20g of magnesium trisilicate grafted with polyethyleneimine, reacting for 2 hours, adding 0.2kg of plasticizer and 10g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting the gas chromatography in standard appendix F of GB 18583 + 2008 'Limited harmful substance in adhesive for interior decoration Material', the TVOC content of an interface treating agent is 33g/L, compared with a sample of a comparative example, the TVOC content is reduced by 29.8%, the compatibility among components is good, the viscosity is 7600mPa & s after being tested by a rotary viscometer, the proper consistency is ensured, no settlement is generated, and the requirement of the environmental protection standard HJ 2541 + 2016 adhesive for environmental marking products is met.
Example 4
Preparing a concrete interface treating agent: firstly, adding 8kg of water into a dissolving kettle, adding 0.3kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.41kg of vinyl acetate into the polymerization kettle, dropwise reacting for 6 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 40g of magnesium trisilicate grafted with polyethyleneimine, reacting for 2 hours, adding 0.2kg of plasticizer and 10g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting the gas chromatography in standard appendix F of GB 18583 + 2008 'Limited harmful substance in adhesive for interior decoration Material', the TVOC content of an interface treating agent is 26g/L, compared with a sample of a comparative example, the TVOC content is reduced by 44.7%, the compatibility among components is good, the viscosity is 11000mPa & s after the test of a rotary viscometer, the proper consistency is ensured, no settlement is generated, and the requirement of the Chinese environmental protection standard HJ 2541 + 2016 adhesive for environmental marking products technical requirements is met.
Example 5
Preparing a concrete interface treating agent: firstly, adding 8kg of water into a dissolving kettle, adding 0.3kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.41kg of vinyl acetate into the polymerization kettle, dropwise reacting for 6 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 80g of magnesium trisilicate grafted with polyethyleneimine, reacting for 2 hours, adding 0.2kg of plasticizer and 10g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting the gas chromatography in standard appendix F of GB 18583 + 2008 'Limited harmful substance in adhesive for interior decoration Material', the TVOC content of an interface treating agent is 21g/L, compared with a sample of a comparative example, the TVOC content is reduced by 55.3%, the compatibility among components is good, the viscosity is 18000mPa & s after being tested by a rotary viscometer, the proper consistency is ensured, no settlement is generated, and the requirement of the Chinese environmental protection standard HJ 2541 + 2016 adhesive for environmental marking products technical requirements is met.
Example 6
Preparing a concrete interface treating agent: firstly, adding 8kg of water into a dissolving kettle, adding 0.3kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.41kg of vinyl acetate into the polymerization kettle, dropwise reacting for 6 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 100g of magnesium trisilicate grafted with polyethyleneimine, reacting for 2 hours, adding 0.2kg of plasticizer and 10g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting the gas chromatography in standard appendix F of GB 18583 + 2008 'Limited harmful substance in adhesive for interior decoration Material', the TVOC content of an interface treating agent is 16g/L, compared with a sample of a comparative example, the TVOC content is reduced by 66%, the compatibility among components is good, the viscosity is 24000mPa & s after being tested by a rotary viscometer, the proper consistency is ensured, no settlement is generated, and the requirement of the Chinese environmental protection standard HJ 2541 + 2016 'adhesive for environmental marking products technical requirements' is met.
Example 7
Preparing a concrete interface treating agent: firstly, adding 9kg of water into a dissolving kettle, adding 0.4kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 30g of ammonium persulfate and 1.2kg of vinyl acetate into the polymerization kettle, dropwise adding for 5 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 50g of magnesium trisilicate grafted with polyethyleneimine, reacting for 1 hour, adding 0.3kg of plasticizer and 15g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting the gas chromatography in standard appendix F of GB 18583 + 2008 "Limit of harmful substance in adhesive for interior decoration Material", the TVOC content of the interface treating agent is 24g/L, compared with the sample of the comparative example, the TVOC content is reduced by 48.9%, the compatibility among the components is good, the viscosity is 16500mPa & s after being tested by a rotary viscometer, the proper consistency is ensured, no settlement is generated, and the requirement of the Chinese environmental protection standard HJ 2541 + 2016 adhesive for environmental Mark product technical requirement is met.
Example 8
Preparing a concrete interface treating agent: adding 7kg of water into a dissolving kettle, adding 0.4kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 20g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.5kg of vinyl acetate into the polymerization kettle, dropwise reacting for 4 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 55g of magnesium trisilicate grafted with polyethyleneimine, reacting for 1 hour, adding 0.4kg of plasticizer and 20g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting the gas phase chromatography in standard appendix F of GB 18583 + 2008 "Limit of harmful substance in adhesive for interior decoration Material", the TVOC content of the interface treating agent is 23g/L, compared with the sample of the comparative example, the TVOC content is reduced by 51.1%, the compatibility among the components is good, the viscosity obtained by the test of a rotary viscometer is 17200 mPa.s, the proper consistency is ensured, no settlement is generated, and the requirement of the Chinese environmental protection standard HJ 2541 + 2016 "adhesive for environmental Mark product technology requirement" is met.
Example 9
Preparing a concrete interface treating agent: firstly, adding 6.5kg of water into a dissolving kettle, adding 0.35kg of polyvinyl alcohol into the dissolving kettle under stirring for dissolving, then sending the dissolved polyvinyl alcohol aqueous solution into a polymerization kettle, adding 30g of emulsifier, stirring uniformly, heating to 70 ℃, uniformly dropwise adding 20g of ammonium persulfate and 1.4kg of vinyl acetate into the polymerization kettle, dropwise adding for reaction for 3 hours, adding 15g of sodium bicarbonate, cooling to 50 ℃, adding 60g of magnesium trisilicate grafted with polyethyleneimine, reacting for 2 hours, adding 0.2kg of plasticizer and 30g of preservative, cooling to room temperature, and discharging to obtain the interface treating agent, wherein the emulsifier is alkoxy polyethylene hydroxyl ethanol, the plasticizer is dipropylene glycol dibenzoate, and the preservative is didecyl dimethyl ammonium chloride.
The Total Volatile Organic Compound (TVOC) content is tested by adopting gas chromatography in standard appendix F of GB 18583 + 2008 ' Limit of harmful substances in adhesive for interior decoration Material, the TVOC content of the interface treating agent is 21g/L, compared with a sample of a comparative example, the TVOC content is reduced by 55.3%, the compatibility among the components is good, the viscosity is 18400mPa & s after being tested by a rotary viscometer, the proper consistency is ensured, no settlement is generated, and the requirement of the environmental protection standard HJ 2541 + 2016 ' adhesive for environmental Mark products technical requirement ' is met.
As can be seen from the above examples and comparative examples, the interface treatment agent prepared by polymerization of the magnesium trisilicate grafted with polyethyleneimine and polyvinyl acetate emulsion has low VOC and excellent viscosity.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (7)
1. An environment-friendly low-VOC interface treating agent is characterized in that the agent is prepared by carrying out polymerization reaction on magnesium trisilicate grafted with polyethyleneimine and polyvinyl acetate emulsion;
the magnesium trisilicate grafted with polyethyleneimine is obtained by reacting polyethyleneimine and magnesium trisilicate under the action of a silane coupling agent;
the silane coupling agent is 3- (methacryloyloxy) propyl trimethoxy silane.
2. The environmentally friendly, low VOC interface treatment according to claim 1, wherein said polyethyleneimine grafted magnesium trisilicate is prepared according to the following method:
A) activating magnesium trisilicate by adopting a silane coupling agent under an acidic condition;
B) reacting the activated magnesium trisilicate obtained in the step A) with polyethyleneimine to obtain the polyethyleneimine grafted magnesium trisilicate.
3. The preparation method of the environment-friendly low-VOC interface treating agent is characterized by comprising the following steps of:
dissolving polyvinyl alcohol in water, adding an emulsifier, ammonium persulfate and vinyl acetate to perform a first polymerization reaction, adding sodium bicarbonate and magnesium trisilicate grafted with polyethyleneimine to perform a second cross-linking polymerization reaction, and finally adding a plasticizer and a preservative to obtain the interface treating agent.
4. The preparation method according to claim 3, wherein the grafted polyethyleneimine magnesium trisilicate, vinyl acetate, polyvinyl alcohol, ammonium persulfate, emulsifier, sodium bicarbonate, water, plasticizer and preservative are in a mass ratio of (0.1-1): (10-30): (3-4): (0.2-0.3): (0.2-0.4): (0.15-0.25): (60-90): (2-4): (0.1-0.3).
5. The method according to claim 3, wherein the emulsifier is an alkoxy polyethylene hydroxy ethanol; the plasticizer is dipropylene glycol dibenzoate; the preservative is didecyl dimethyl ammonium chloride.
6. The preparation method according to claim 3, wherein the temperature of the first polymerization reaction is 70 ℃ and the reaction time is 3-6 h.
7. The preparation method according to claim 3, wherein the temperature of the second cross-linking polymerization reaction is 50 ℃ and the reaction time is 1-2 h.
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