一种有机硅混凝土防护剂及其制备方法

本发明涉及一种有机硅混凝土防护剂及其制备方法，属混凝土添加制剂技术领域。该防护剂是将烷基硅烷低聚体、乳化剂、氨基硅烷增粘剂、水加入混合器中搅拌，搅拌温度为50～70℃，搅拌时间为2～4小时，冷却至常温后得到有机硅混凝土防护剂。本发明由于烷基硅烷低聚体的分子结构小、渗透性强，能有效渗入混凝土内部，并与混凝土吸收的水份迅速交联聚合成大分子硅氧烷，不阻塞混凝土结构中的毛细管和孔隙，空气及水气能够自由进出，使混凝土具有良好的增水性和透气性。解决了现有混凝土防护剂在表面形成大分子有机物涂膜，当混凝土受到高温时防护剂涂层易出现鼓泡、龟裂、起皮、剥离脱落的问题。大大提高了混凝土材料的使用寿命。

技术领域

Technical field:

The present invention relates to a kind of organosilicon concrete protectant and preparation method thereof, belong to concrete and add the preparation technique field.

背景技术

Background technology:

Concrete is a kind of porous material, portion exists kapillary, hole and the bubble that varies in size within it, can absorb air outside and moisture content in a large number, if long-term exposure is in rugged environments such as topsoil, ultraviolet ray, acid rain, be easy to suffer outside atmosphere to corrode and damage, therefore concrete protective treatment more and more is subject to people's attention.

At present; domestic available coagulation soil protective agent has coating, ointment, pitch etc. usually; the protection principle of this class protective agent is by at the certain thickness above-mentioned protective agent of concrete surface brushing one deck; making it form macromolecular organism at concrete surface films; come the hole of closed concrete material surface by this layer organic coating film; make its invasion that is not subjected to extraneous hazardous medium, reach the purpose of protection concrete structure.

Mainly there are two shortcomings in the concrete protection technology of this quasi-tradition: the one, because the concrete surface hole is blocked by larger molecular organics matter, make concrete airtight, when concrete is exposed in the atmospheric environment, be subjected to that sunlight tans by the sun or the influence of other hot conditions, air in the hole of inside concrete and the kapillary will be overflowed by expanded by heating internally, will cause concrete surface protective agent coating bubbling, be full of cracks, peeling to occur like this, peel off phenomenon such as come off; Not only directly cause protective agent to lose the protection effect, but also influence the attractive in appearance of protective agent coating, peel off the larger molecular organics that comes off and in environment, be not easy degraded, contaminate environment; The 2nd, because this class protective agent is larger molecular organics, perviousness is very poor, can only can't penetrate into inside concrete attached to concrete surface, in case the therefore top coat phenomenons such as bubbling, be full of cracks, peeling occur that is damaged has just lost the protection effect.

发明内容

Summary of the invention:

The objective of the invention is to: provide that a kind of molecular structure is little, perviousness is strong, can effectively infiltrate inside concrete 5～10mm, and become the macromole siloxanes with the rapid crosslinking polymerization of moisture content generation chemical reaction that concrete absorbs, have excellent waterproofness, ventilation property, perviousness, long-lasting; Film at surface formation larger molecular organics to solve the employing of existing concrete protective agent, the surface pore is blocked by larger molecular organics matter when concrete is subjected to high temperature, cause the protective agent coating bubbling, be full of cracks, peeling to occur, peel off and come off, lose organosilicon concrete protectant of protection efficacy problems and preparation method thereof.

The present invention realizes above-mentioned purpose by the following technical solutions:

A kind of organosilicon concrete protectant is characterized in that: it is made by following weight percentages:

Alkyl silane oligomer 15～30%; Emulsifying agent 2～10%;

Aminosilane tackifier 3～10%; Water 50～80%.

The ratio range for preparing preferred weight percent of the present invention is:

Alkyl silane oligomer 18～25%; Emulsifying agent 4～8%;

Aminosilane tackifier 4～7%; Water 60～70%.

The proportioning of optimum weight per-cent of the present invention is:

Alkyl silane oligomer 20%; Emulsifying agent 5%;

Aminosilane tackifier 5%; Water 70%.

Described alkyl silane oligomer is made by following weight percentages:

Methyl-propyl diethoxy silane 6.8%; N-propyl triethoxy 13.5%;

Chain alkyl triethoxyl silane 13.5%; Tetraethoxysilane 6.8%;

Concentrated hydrochloric acid 13.5%; Distilled water 32.4%;

Ethanol 13.5%.

Wherein, chain alkyl triethoxyl silane general formula is RSi (OCH ₂CH ₃) ₃, R is C _6～18Alkyl group.

Described aminosilane tackifier are any one in γ-An Bingjisanyiyangjiguiwan, γ-aminopropyl methyldiethoxysilane, N-(β-aminoethyl)-γ-An Bingjisanyiyangjiguiwan, N-(β-aminoethyl)-γ-aminopropyl methyldiethoxysilane, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan, N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane.

Described emulsifying agent is any one in dodecyl sodium sulfonate calcium, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, the calcium dodecylbenzene sulphonate.

The preparation method of above-mentioned organosilicon concrete protectant is as follows:

The first step: produce the alkyl silane oligomer earlier, the preparation method of alkyl silane oligomer is as follows:

A, that concentrated hydrochloric acid and distilled water are mixed the mixed solution of making concentrated hydrochloric acid and distilled water is stand-by;

B, in the reactor that has heating, stirring, reflux, add methyl-propyl diethoxy silane, n-propyl triethoxy, chain alkyl triethoxyl silane, tetraethoxysilane, ethanol and heat temperature raising successively;

C, when temperature rises to 70～80 ℃, the mixed solution of concentrated hydrochloric acid and distilled water slowly is added drop-wise in the reactor, stir fast with 150 rev/mins speed, reacted 6～8 hours;

After D, stirring reaction were finished, decompression steamed the ethanol of etoh solvent and reaction generation, is cooled to below 40 ℃ with tap water, carries out suction filtration then, obtains the alkyl silane oligomer.

Second step: the alkyl silane oligomer, aminosilane tackifier, emulsifying agent and the water that make are added in the mixing tank of being with whipping appts successively, speed with 150 rev/mins stirs fast, be warming up to 50～70 ℃ of stirring reactions then 2～4 hours, be cooled to normal temperature with tap water after reaction finishes, promptly obtain organosilicon concrete protectant.

The invention has the advantages that: the alkyl silane oligomer among the present invention is because its molecular structure is little, the characteristics that perviousness is strong, can effectively infiltrate inside concrete 5～10mm, and with moisture content generation chemical reaction that concrete absorbs after rapidly crosslinking polymerization become the macromole siloxanes, alkyl in the siloxane molecule is arranged at the concrete material surface orientation, can give concrete material good hydrophobicity by organically-modified, thereby from outside to inside at concrete surface and the firm barrier of surging of inner formation, reduce the water-intake rate of concrete material, make moisture content be difficult to infiltrate concrete, improve the work-ing life of concrete material greatly.Particularly this class organosilicon protective agent carries out the self-crosslinking polymerization at concrete surface and inner kapillary and the inwall of hole, do not block kapillary and hole in the concrete structure, air and aqueous vapor can free in and out, and give concrete and have air permeability and good.

After n-propyl triethoxy and chain alkyl triethoxyl silane solidified, chain alkyl can give concrete surface good hydrophobicity, makes concrete surface have low water absorption; And the short propyl group of chain can be given the protective agent good penetration, makes protective agent porous of the present invention advance inside concrete, can continue the performance protective effect for a long time, and it is long-lasting that protective agent of the present invention is had.

The methyl-propyl diethoxy silane can give protective agent film forming silicone resin favorable linearity, make resin behind the concrete surface crosslinking curing, have good snappiness and elasticity, reduce protective agent of the present invention aging phenomenon that be full of cracks, peeling occur in environment.

Tetraethoxysilane, aminosilane can quicken the film forming alkyl silane oligomer of protective agent crosslinking curing, make protective agent of the present invention rapid crosslinking curing performance protection effect after use.

附图说明null实施方式

Embodiment:

Embodiment 1:

It is stand-by that 13.5 kilograms of concentrated hydrochloric acids (massfraction 35%) and 32.4 kilograms of distilled water are mixed the mixed solution of making concentrated hydrochloric acid and distilled water.In the reactor that has heating, stirring, reflux, add 6.8 kilograms of methyl-propyl diethoxy silanes, 13.5 kilograms of n-propyl triethoxies, 13.5 kilograms of chain alkyl triethoxyl silanes, 6.8 kilograms of tetraethoxysilanes and 13.5 kilograms of ethanol and heat temperature raising successively.When temperature rises to 75 ℃, the mixed solution of concentrated hydrochloric acid and distilled water slowly is added drop-wise in the reactor, stir fast with 150 rev/mins speed, reacted 6～8 hours; After stirring reaction was finished, decompression steamed the ethanol of etoh solvent and reaction generation, is cooled to below 40 ℃ with tap water, carries out suction filtration then, obtains the alkyl silane oligomer.

In the mixing tank of band whipping appts, add 15 kilograms of alkyl silane oligomers, 3 kilograms of γ-An Bingjisanyiyangjiguiwans, 2 kilograms of dodecyl sodium sulfonate calcium and 80 kilograms in water and evenly stirring successively, whipping temp is 55 ℃, churning time is 3.5 hours, obtains organosilicon concrete protectant after being cooled to normal temperature.

Embodiment 2:

It is stand-by that 13.5 kilograms of concentrated hydrochloric acids (massfraction 35%) and 32.4 kilograms of distilled water are mixed the mixed solution of making concentrated hydrochloric acid and distilled water.In the reactor that has heating, stirring, reflux, add 6.8 kilograms of methyl-propyl diethoxy silanes, 13.5 kilograms of n-propyl triethoxies, 13.5 kilograms of chain alkyl triethoxyl silanes, 6.8 kilograms of tetraethoxysilanes and 13.5 kilograms of ethanol and heat temperature raising successively; When temperature rises to 75 ℃, the mixed solution of concentrated hydrochloric acid and distilled water slowly is added drop-wise in the reactor, stir fast with 150 rev/mins speed, reacted 6～8 hours; After stirring reaction was finished, decompression steamed the ethanol of etoh solvent and reaction generation, is cooled to below 40 ℃ with tap water, carries out suction filtration then, obtains the alkyl silane oligomer.

In the mixing tank of band whipping appts, add 22 kilograms of alkyl silane oligomers, N-(β-aminoethyl)-γ-6 kilograms of aminopropyl methyl dimethoxysilanes, 6 kilograms of Sodium dodecylbenzene sulfonatees and 66 kilograms in water and evenly stirring successively, whipping temp is 60 ℃, churning time is 3 hours, obtains organosilicon concrete protectant after the cooling.

Embodiment 3

It is stand-by that 13.5 kilograms of concentrated hydrochloric acids (massfraction 35%) and 32.4 kilograms of distilled water are mixed the mixed solution of making concentrated hydrochloric acid and distilled water.In the reactor that has heating, stirring, reflux, add 6.8 kilograms of methyl-propyl diethoxy silanes, 13.5 kilograms of n-propyl triethoxies, 13.5 kilograms of chain alkyl triethoxyl silanes, 6.8 kilograms of tetraethoxysilanes and 13.5 kilograms of ethanol and heat temperature raising successively; When temperature rises to 75 ℃, the mixed solution of concentrated hydrochloric acid and distilled water slowly is added drop-wise in the reactor, stir fast with 150 rev/mins speed, reacted 6～8 hours; After stirring reaction was finished, decompression steamed the ethanol of etoh solvent and reaction generation, is cooled to below 40 ℃ with tap water, carries out suction filtration then, obtains the alkyl silane oligomer.

In the mixing tank of band whipping appts, add 20 kilograms of alkyl silane oligomers, N-(β-aminoethyl)-5 kilograms of γ-An Bingjisanjiayangjiguiwans, 5 kilograms of sodium laurylsulfonates and 70 kilograms in water and evenly stirring successively, whipping temp is 65 ℃, churning time is 2.5 hours, obtains organosilicon concrete protectant after the cooling.