CN105669080A - Preparation method of organosilicon cement waterproof agent capable of realizing self-repairing of cracks - Google Patents

Abstract

The invention discloses a preparation method of an organosilicon cement waterproof agent capable of realizing self-repairing of cracks and belongs to the technical field of preparation of a waterproof agent. Prepared calcium silicate is taken as a seed crystal and then added to organosilicon waterproofing mixed slurry, vacuum freeze drying is performed after rotary evaporateion concentration, a product is supplemented by a complexing agent, mechanical lapping and activation are performed, and operation of the preparation method of the organosilicon cement waterproof agent capable of realizing self-repairing of the cracks is completed. Examples prove that the preparation method is simple and easy to operate, the water reduction amount of the prepared waterproof agent is large, the plasticity-maintaining time is long, the organosilicon cement waterproof agent enters pores in concrete through water-seepage channels under the action of water or through the normal capillary action of concrete and has a hydration reaction with cement particles unhydrated in the concrete, compact hydrated crystals are formed and block pores, capillary tubes and cracks of the concrete, the waterproof purpose is achieved, and the waterproof property is gradually enhanced with time due to the self-repairing performance.

Description

A kind of can the preparation method of selfreparing crack organosilicon cement water-resisting agent

Technical field

The present invention disclose a kind of can the preparation method of selfreparing crack organosilicon cement water-resisting agent, belong to water-resisting agent preparing technical field.

Background technology

Water is the important substance causing cement concrete constructions and reinforced concrete structure durability to damage, it is no matter the soft water erosion of cement concrete, freeze-thaw damage, alkali, steel bar corrosion, the corrosion of even water conservancy project, Accommodation, all it be unable to do without the effect of water, the participation not having water, major part corrodes and almost can not occur. Therefore, waterproof is the important measures improving cement concrete constructions weather resistance, or even essential measure.

Waterproofing agent of organosilicon is the new and effective water-proof material of a kind of pollution-free, nonirritant, for the widespread use of advanced country in the world institute, this product spraying (or brushing) is after building surface, can its surface formed naked eyes be not aware of one layer of water white transparency, uvioresistant air-permeating film, when rainwater is blown and beaten on it or during wet wet air, water droplet can trickle by nature, moisture is stoped to invade, building surface dust can also be washed away totally simultaneously, thus play and make interior wall protection against the tide, mildew-resistant, exterior wall cleaning and prevent the effects such as weathering.

At present, domestic common water-based organic silicon waterproof agent divides two classes: one, be strong basicity, and after brushing, the meeting accumulation of salt in the surface soil, directly affects outward appearance and waterproof life-span, have certain action of rust; Two, being type of latex type, the water-resisting agent quality guaranteed period is short, and waterproof effect is not obvious, two brushing property differences; In addition, traditional water-resisting agent water resistance is poor, it is few to subtract the water yield, protects that to mould the time long, sometimes need disastrously to add the admixture such as pumping agent, water reducer, it may also be useful to loaded down with trivial details, though being very effective in the starting stage, but prolongation in time, its performance is degenerated gradually and is lost waterproof effect.

Summary of the invention

The technical problem that the present invention mainly solves: though very effective in the starting stage for water-resisting agent traditional at present, but the prolongation along with the time, performance degradation and lose waterproof effect, cause that water resistance is poor, to subtract the water yield few, it is long that guarantor moulds the time, operate loaded down with trivial details present situation, provide a kind of using obtained Calucium Silicate powder as crystal seed, add in organic silicon water-proofing mixed slurry afterwards, concentrated by rotary evaporation final vacuum freeze-drying, being aided with complexing agent, mechanical mill activates, thus obtain can the method for selfreparing crack organosilicon cement water-resisting agent. Operation is simple for the method, the water-resisting agent made subtract the water yield big, protect that to mould the time long, entered in the hole of inside concrete under the effect of water by the normal wicking action of penetrating passage or concrete, with cement granules generation hydration reaction unhydrated in concrete, form fine and close aquation crystal, hole, the kapillary of blocking concrete and carefully stitch, reach waterproof object, and the self-healing properties having makes water-repellancy strengthen gradually in time.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

(1) measuring the saturated aqua calcis of 80～100mL loads in 500mL plastic cement bottle, it is placed on magnetic stirrer to stir, the process stirred is dripped points for 2～4 times add 20～30mL concentration is the sodium silicate solution of 0.2mol/L, after dropwising, plastic cement bottle is sealed, put into vortex oscillator, after the oscillation of power 10～15min of 20～30W, to leave standstill 2～3 days in the ice-water bath of 4～6 DEG C;

(2) after leaving standstill end, being filtered by mixed solution, separation obtains filter residue, pours in agate mortar with after vacuum drier drying by filter residue, grinds to form powder and crosses 200 mesh standard sieves, obtains Calucium Silicate powder powder, for subsequent use;

(3) in the high-temperature high-pressure reaction kettle of 10L, 1～2L containing hydrogen silicone oil, 2～3L dehydrated alcohol and 300～500g potassium hydroxide powder is poured into, startup agitator carries out stirring and opens steam valve, leads to the water vapor insulation reaction 2～4h of temperature between 90～100 DEG C inwards;

(4) reaction continues to add 10～20g organo-silicone rubber particle, 3～5g calcium lignin sulphonate and 50～100mL Glacial acetic acid in reactor after terminating, reduce temperature in the kettle to 70～80 DEG C, it is pressurized to 0.3～0.5MPa, after continuing stirring reaction 3～5h, make discharging after its naturally cooling, obtain thick product;

(5) thick product obtained above is put into rotatory evaporator, raised temperature to 40～50 DEG C, concentrated by rotary evaporation to the 2/3 of thick product original volume, then by above-mentioned Calucium Silicate powder powder for subsequent use and concentrated after thick product be that 1:3 mixes by solid-to-liquid ratio, obtain mixed solution;

(6) above-mentioned mixed solution is put into ultrasonic disperse instrument, with 25～35KHz, the power ultrasonic dispersion 1～2h of 100～200W, Calucium Silicate powder powder is dispersed in concentrated solution uniformly, and moved into vacuum-freeze-dry machine and carry out lyophilize, first pulverize 80 mesh standard sieves with micronizer mill after dry, obtain granular product;

(7) take the above-mentioned obtained granular product of 100～200g and put into corundum mortar, continue to add the amine front three fork sodium phosphate of granular product cumulative volume 5～10%, grinding 2～3h, make both fully mix and after activating, pack, pack and obtain a kind of can selfreparing crack organosilicon cement water-resisting agent.

The application method of the present invention is: the silicon cement waterproof agent that has the present invention obtained mixes in cement concrete, wherein incorporation is the 2～4% of cement concrete quality, mix, waterproof action can be played, do not need again to add the admixture such as pumping agent, water reducer, easy to operate, there is water resistance good, subtract the water yield big, protect the feature moulding time length, it is possible to be widely used in having the concrete works of water proof anti-seepage requirement.

The invention has the beneficial effects as follows:

(1) the present invention is simple to operate, and the organosilicon cement water-resisting agent made can play waterproof action, does not need again to add the admixture such as pumping agent, water reducer, and easy to operate to subtract the water yield big, it is long that guarantor moulds the time;

(2) the organosilicon cement water-resisting agent that the present invention obtains has self-healing performance so that water-repellancy strengthens in time gradually.

Embodiment

First measuring the saturated aqua calcis of 80～100mL loads in 500mL plastic cement bottle, it is placed on magnetic stirrer to stir, the process stirred is dripped points for 2～4 times add 20～30mL concentration is the sodium silicate solution of 0.2mol/L, after dropwising, plastic cement bottle is sealed, put into vortex oscillator, after the oscillation of power 10～15min of 20～30W, to leave standstill 2～3 days in the ice-water bath of 4～6 DEG C; Then leaving standstill after terminating, filtered by mixed solution, separation obtains filter residue, pours in agate mortar with after vacuum drier drying by filter residue, grinds to form powder and crosses 200 mesh standard sieves, and obtained Calucium Silicate powder powder is for subsequent use; Subsequently to the high-temperature high-pressure reaction kettle of 10L is poured into 1～2L containing hydrogen silicone oil, 2～3L dehydrated alcohol and 300～500g potassium hydroxide powder, startup agitator carries out stirring and opens steam valve, leads to the water vapor insulation reaction 2～4h of temperature between 90～100 DEG C inwards;Reaction afterwards continues to add 10～20g organo-silicone rubber particle, 3～5g calcium lignin sulphonate and 50～100mL Glacial acetic acid in reactor after terminating, reduce temperature in the kettle to 70～80 DEG C, it is pressurized to 0.3～0.5MPa, after continuing stirring reaction 3～5h, make discharging after its naturally cooling, obtain thick product; Next thick product obtained above is put into rotatory evaporator, raised temperature to 40～50 DEG C, concentrated by rotary evaporation to the 2/3 of thick product original volume, then by above-mentioned Calucium Silicate powder powder for subsequent use and concentrated after thick product be that 1:3 mixes by solid-to-liquid ratio, obtain mixed solution; Above-mentioned mixed solution is put into ultrasonic disperse instrument, with 25～35KHz, the power ultrasonic dispersion 1～2h of 100～200W, Calucium Silicate powder powder is dispersed in concentrated solution uniformly, and moved into vacuum-freeze-dry machine and carry out lyophilize, first pulverize 80 mesh standard sieves with micronizer mill after dry, obtain granular product; Finally take the above-mentioned obtained granular product of 100～200g and put into corundum mortar, continue to add the amine front three fork sodium phosphate of granular product cumulative volume 5～10%, grinding 2～3h, make both fully mix and after activating, pack, pack and obtain a kind of can selfreparing crack organosilicon cement water-resisting agent.

Example 1

First measuring the saturated aqua calcis of 80mL loads in 500mL plastic cement bottle, it is placed on magnetic stirrer to stir, the process stirred is divided drip for 2 times and add the sodium silicate solution that 20mL concentration is 0.2mol/L, after dropwising, plastic cement bottle is sealed, put into vortex oscillator, after the oscillation of power 10min of 20W, to leave standstill 2 days in the ice-water bath of 4 DEG C; Then leaving standstill after terminating, filtered by mixed solution, separation obtains filter residue, pours in agate mortar with after vacuum drier drying by filter residue, grinds to form powder and crosses 200 mesh standard sieves, and obtained Calucium Silicate powder powder is for subsequent use; Subsequently to pouring 1L containing hydrogen silicone oil, 2L dehydrated alcohol and 300g potassium hydroxide powder in the high-temperature high-pressure reaction kettle of 10L into, startup agitator carries out stirring and opens steam valve, leads to the water vapor insulation reaction 2h of temperature between 90 DEG C inwards; Reaction afterwards continues to add 10g organo-silicone rubber particle, 3g calcium lignin sulphonate and 50mL Glacial acetic acid in reactor after terminating, and reduces temperature in the kettle to 70 DEG C, is pressurized to 0.3MPa, after continuing stirring reaction 3h so that it is discharging after naturally cooling, obtains thick product; Next thick product obtained above is put into rotatory evaporator, raised temperature to 40 DEG C, concentrated by rotary evaporation to the 2/3 of thick product original volume, then by above-mentioned Calucium Silicate powder powder for subsequent use and concentrated after thick product be that 1:3 mixes by solid-to-liquid ratio, obtain mixed solution;

Above-mentioned mixed solution is put into ultrasonic disperse instrument, with the power ultrasonic of 25KHz, 100W dispersion 1h, Calucium Silicate powder powder is dispersed in concentrated solution uniformly, and moved into vacuum-freeze-dry machine and carry out lyophilize, first pulverize 80 mesh standard sieves with micronizer mill after dry, obtain granular product; Finally take the above-mentioned obtained granular product of 100g and put into corundum mortar, continue to add the amine front three fork sodium phosphate of granular product cumulative volume 5%, grinding 2h, make both fully mix and after activating, pack, pack and obtain a kind of can selfreparing crack organosilicon cement water-resisting agent.

This case method is unique novel, it may also be useful to time, the silicon cement waterproof agent that has the present invention obtained mixes in cement concrete, wherein incorporation is the 2% of cement concrete quality, mix, waterproof action can be played, do not need again to add the admixture such as pumping agent, water reducer, easy to operate, there is water resistance good, subtract the water yield big, protect the feature moulding time length, it is possible to be widely used in having the concrete works of water proof anti-seepage requirement.

Example 2

First measuring the saturated aqua calcis of 90mL loads in 500mL plastic cement bottle, it is placed on magnetic stirrer to stir, the process stirred is divided drip for 3 times and add the sodium silicate solution that 25mL concentration is 0.2mol/L, after dropwising, plastic cement bottle is sealed, put into vortex oscillator, after the oscillation of power 13min of 25W, to leave standstill 2.5 days in the ice-water bath of 5 DEG C; Then leaving standstill after terminating, filtered by mixed solution, separation obtains filter residue, pours in agate mortar with after vacuum drier drying by filter residue, grinds to form powder and crosses 200 mesh standard sieves, and obtained Calucium Silicate powder powder is for subsequent use; Subsequently to pouring 1.5L containing hydrogen silicone oil, 2.5L dehydrated alcohol and 400g potassium hydroxide powder in the high-temperature high-pressure reaction kettle of 10L into, startup agitator carries out stirring and opens steam valve, leads to the water vapor insulation reaction 3h of temperature between 95 DEG C inwards; Reaction afterwards continues to add 15g organo-silicone rubber particle, 4g calcium lignin sulphonate and 80mL Glacial acetic acid in reactor after terminating, and reduces temperature in the kettle to 75 DEG C, is pressurized to 0.4MPa, after continuing stirring reaction 4h so that it is discharging after naturally cooling, obtains thick product; Next thick product obtained above is put into rotatory evaporator, raised temperature to 45 DEG C, concentrated by rotary evaporation to the 2/3 of thick product original volume, then by above-mentioned Calucium Silicate powder powder for subsequent use and concentrated after thick product be that 1:3 mixes by solid-to-liquid ratio, obtain mixed solution; Above-mentioned mixed solution is put into ultrasonic disperse instrument, with the power ultrasonic of 30KHz, 150W dispersion 1.5h, Calucium Silicate powder powder is dispersed in concentrated solution uniformly, and moved into vacuum-freeze-dry machine and carry out lyophilize, first pulverize 80 mesh standard sieves with micronizer mill after dry, obtain granular product; Finally take the above-mentioned obtained granular product of 150g and put into corundum mortar, continue to add the amine front three fork sodium phosphate of granular product cumulative volume 8%, grinding 2.5h, make both fully mix and after activating, pack, pack and obtain a kind of can selfreparing crack organosilicon cement water-resisting agent.

This case method is unique novel, it may also be useful to time, the silicon cement waterproof agent that has the present invention obtained mixes in cement concrete, wherein incorporation is the 3% of cement concrete quality, mix, waterproof action can be played, do not need again to add the admixture such as pumping agent, water reducer, easy to operate, there is water resistance good, subtract the water yield big, protect the feature moulding time length, it is possible to be widely used in having the concrete works of water proof anti-seepage requirement.

Example 3

First measuring the saturated aqua calcis of 100mL loads in 500mL plastic cement bottle, it is placed on magnetic stirrer to stir, the process stirred is divided drip for 4 times and add the sodium silicate solution that 30mL concentration is 0.2mol/L, after dropwising, plastic cement bottle is sealed, put into vortex oscillator, after the oscillation of power 15min of 30W, to leave standstill 3 days in the ice-water bath of 6 DEG C; Then leaving standstill after terminating, filtered by mixed solution, separation obtains filter residue, pours in agate mortar with after vacuum drier drying by filter residue, grinds to form powder and crosses 200 mesh standard sieves, and obtained Calucium Silicate powder powder is for subsequent use; Subsequently to pouring 2L containing hydrogen silicone oil, 3L dehydrated alcohol and 500g potassium hydroxide powder in the high-temperature high-pressure reaction kettle of 10L into, startup agitator carries out stirring and opens steam valve, leads to the water vapor insulation reaction 4h of temperature between 100 DEG C inwards; Reaction afterwards continues to add 20g organo-silicone rubber particle, 5g calcium lignin sulphonate and 100mL Glacial acetic acid in reactor after terminating, and reduces temperature in the kettle to 80 DEG C, is pressurized to 0.5MPa, after continuing stirring reaction 5h so that it is discharging after naturally cooling, obtains thick product;Next thick product obtained above is put into rotatory evaporator, raised temperature to 50 DEG C, concentrated by rotary evaporation to the 2/3 of thick product original volume, then by above-mentioned Calucium Silicate powder powder for subsequent use and concentrated after thick product be that 1:3 mixes by solid-to-liquid ratio, obtain mixed solution;

Above-mentioned mixed solution is put into ultrasonic disperse instrument, with the power ultrasonic of 35KHz, 200W dispersion 2h, Calucium Silicate powder powder is dispersed in concentrated solution uniformly, and moved into vacuum-freeze-dry machine and carry out lyophilize, first pulverize 80 mesh standard sieves with micronizer mill after dry, obtain granular product; Finally take the above-mentioned obtained granular product of 200g and put into corundum mortar, continue to add the amine front three fork sodium phosphate of granular product cumulative volume 10%, grinding 3h, make both fully mix and after activating, pack, pack and obtain a kind of can selfreparing crack organosilicon cement water-resisting agent.

This case method is unique novel, it may also be useful to time, the silicon cement waterproof agent that has the present invention obtained mixes in cement concrete, wherein incorporation is the 4% of cement concrete quality, mix, waterproof action can be played, do not need again to add the admixture such as pumping agent, water reducer, easy to operate, there is water resistance good, subtract the water yield big, protect the feature moulding time length, it is possible to be widely used in having the concrete works of water proof anti-seepage requirement.

Claims (1)

1. one kind can the preparation method of selfreparing crack organosilicon cement water-resisting agent, it is characterised in that concrete preparation process is:

(1) measuring the saturated aqua calcis of 80～100mL loads in 500mL plastic cement bottle, it is placed on magnetic stirrer to stir, the process stirred is dripped points for 2～4 times add 20～30mL concentration is the sodium silicate solution of 0.2mol/L, after dropwising, plastic cement bottle is sealed, put into vortex oscillator, after the oscillation of power 10～15min of 20～30W, to leave standstill 2～3 days in the ice-water bath of 4～6 DEG C;

(2) after leaving standstill end, being filtered by mixed solution, separation obtains filter residue, pours in agate mortar with after vacuum drier drying by filter residue, grinds to form powder and crosses 200 mesh standard sieves, obtains Calucium Silicate powder powder, for subsequent use;

(3) in the high-temperature high-pressure reaction kettle of 10L, 1～2L containing hydrogen silicone oil, 2～3L dehydrated alcohol and 300～500g potassium hydroxide powder is poured into, startup agitator carries out stirring and opens steam valve, leads to the water vapor insulation reaction 2～4h of temperature between 90～100 DEG C inwards;

(4) reaction continues to add 10～20g organo-silicone rubber particle, 3～5g calcium lignin sulphonate and 50～100mL Glacial acetic acid in reactor after terminating, reduce temperature in the kettle to 70～80 DEG C, it is pressurized to 0.3～0.5MPa, after continuing stirring reaction 3～5h, make discharging after its naturally cooling, obtain thick product;

(5) thick product obtained above is put into rotatory evaporator, raised temperature to 40～50 DEG C, concentrated by rotary evaporation to the 2/3 of thick product original volume, then by above-mentioned Calucium Silicate powder powder for subsequent use and concentrated after thick product be that 1:3 mixes by solid-to-liquid ratio, obtain mixed solution;

(6) above-mentioned mixed solution is put into ultrasonic disperse instrument, with 25～35KHz, the power ultrasonic dispersion 1～2h of 100～200W, Calucium Silicate powder powder is dispersed in concentrated solution uniformly, and moved into vacuum-freeze-dry machine and carry out lyophilize, first pulverize 80 mesh standard sieves with micronizer mill after dry, obtain granular product;

(7) take the above-mentioned obtained granular product of 100～200g and put into corundum mortar, continue to add the amine front three fork sodium phosphate of granular product cumulative volume 5～10%, grinding 2～3h, make both fully mix and after activating, pack, pack and obtain a kind of can selfreparing crack organosilicon cement water-resisting agent.