A kind of recoverying and utilizing method of organosilicon slag slurry
Technical field
The invention belongs to environmental protection technical field, specifically a kind of recoverying and utilizing method of organosilicon slag slurry.
Background technology
In recent years, as expanding economy, the quickening of process of industrialization and the raising of the level of urbanization, facing mankind
Increasing environmental pressure, various solid wastes caused by industrial processes and urban construction, which are removed, remakes solid waste brought etc.
The living environment of resident is annoying always, it is broken to change this ecological balance.
Wherein, organosilicon slag slurry is exactly a kind of more serious waste of pollution, and it is produced in organic silicon monomer building-up process
A kind of raw waste residue slurry, it accounts for amount of monomer about 3%, and with the rapidly extension of organic silicon monomer yield, supervening largely has
Machine silicon waste residue slurry, its mainly form be brought out by more high-boiling components and a small amount of fluid bed silica flour (particle diameter 2~
150um), copper powder and micro- Fe, Zn, Al, Sn etc..70.5~250 DEG C of high-boiling components boiling range therein, composition are mainly two silicon
Alkane, siloxanes, silicon support alkane, solid content is 20~75%.If be exposed in air, easily cause strong acid mist and burning,
Therefore, it is necessary to harmless treatment is carried out to it.
As silicone industry develops rapidly, organosilicon chlorosilane monomer yield is also increasing, and organosilicon high-boiling product is
One of accessory substance of organosilicon chlorosilane monomer production, main source has two kinds:First, pass through rectifying organosilicon chlorosilane monomer
Obtain, the type high-boiling components account for 5% of chlorosilane monomer or so, are easier to carry out commercial development utilization;Two be derived from it is organic
Silicon slurry, the type high-boiling components account for 3~5% of monomer capacity or so, complicated component, and carry the solids such as a large amount of silicon, copper secretly
Grain material, generation corrosivity hydrogen chloride gas is easily reacted with moisture in air, can not be handled with simple method.
The content of the invention
The present invention is precisely in order to solve the above problems, there is provided a kind of recoverying and utilizing method of organic silicon waste residue slurry, realizes
The cyclic utilization of waste, reduce the pollution to environment, meet strategy of sustainable development requirement.
The technical scheme is that:A kind of recoverying and utilizing method of organosilicon slag slurry, comprises the following steps:
(1) low-boiling-point substance of addition 23~48% is hydrolyzed in organosilicon slag slurry, and the low-boiling-point substance is chloromethanes, tetramethyl
Any one in base silicon or trichlorosilane or two or more any combination, for temperature control at 45~47 DEG C, use is low during hydrolysis
Fast 20~30r/min of mixer stirrings, 3~7h of hydrolysis, carries out separation of solid and liquid with solid-liquid separator by the product after hydrolysis, obtains
Supernatant and sediment, supernatant are flowed out from the upper end of solid-liquid separator, and sediment is discharged from the bottom of solid-liquid separator;
(2) supernatant that sub-argument goes out carries out alcoholysis with ethanol, and ethanol consumption is the 30~40% of supernatant, and glycolysis temperature is
40~45 DEG C, the alcoholysis time is 0.5~1h, and bottom sediment carries out alkaline hydrolysis with alkali lye, and the alkali lye is sodium hydroxide or hydrogen-oxygen
Change potassium, dosage is the 20~40% of sediment, and the alkaline hydrolysis time is 2~3h, and it is 7.5~8.0 to keep final pH;
(3) final product of alcoholysis and alkaline hydrolysis is fully incorporated sedimentation basin in step (2), with 12~15% Klorvess Liquid
Washed, obtain final dilution and dry slag, dry slag is dehydrated, it is stand-by;
(4) cement mortar is prepared together with above-mentioned dry slag and cement and sand, wherein, dry slag 8~15%, cement 28~
32%, surplus is sand, after dry-mixed, then mixes 1.3~2.5% dilution, adds water to be prepared into cement mortar for building, product tool
Have with good hydrophobicity, prevent from staiing;
(5) it is 68~70% above-mentioned dilution to be concentrated into water content, mixes with organic solvent, adds under agitation
48~58% aliphatic acid is reacted, about 50~90 DEG C of reaction temperature, the reactant that reaction finishes is collected, on demand
Add water and be configured to construction material waterproofing agent, the material handled through waterproofing agent of the present invention has good gas permeability, has certain
Corrosion resistance, extend Building life cycle.
Further, in such scheme, the concentration of the ethanol is 50~65%, with ethanol part can be made less soluble
The silanol of solution is dissolved into ethanol, to adjust methane-siliconic acid sodium content.
Further, in such scheme, the mass fraction of the alkali lye is 32~40%, can be by bottom precipitation with alkali
In the high-boiling components that contain fully dissolve.
Further, in such scheme, the organic solvent is chloroform or phenol, its dosage for dilution 3~
10%, organic solvent can promote the progress of reaction.
Further, in such scheme, the aliphatic acid is polyunsaturated fatty acid, can using polyunsaturated fatty acid
To strengthen the waterproof effect of final product.
Beneficial effects of the present invention are:The organosilicon slag slurry recoverying and utilizing method simple possible of the present invention, it is dry after hydrolysis
Slag can be used to prepare cement mortar, and product prevents from staiing with good hydrophobicity;Dilution liquid energy is made construction material and prevented
Aqua, the material handled through waterproofing agent of the present invention have good gas permeability, there is certain corrosion resistance, extend the building longevity
Life;Fully recycling for waste is realized, reduces the pollution to environment, meets strategy of sustainable development requirement.
Embodiment
Embodiment 1:A kind of recoverying and utilizing method of organosilicon slag slurry, comprises the following steps:
(1) low-boiling-point substance of addition 23% is hydrolyzed in organosilicon slag slurry, and the low-boiling-point substance is chloromethanes, tetramethylsilane
Or any one in trichlorosilane or two or more any combination, temperature control uses low-speed mixer at 45 DEG C during hydrolysis
20r/min stirring hydrolysis 3h, carry out separation of solid and liquid with solid-liquid separator by the product after hydrolysis, obtain supernatant and sediment,
Supernatant is flowed out from the upper end of solid-liquid separator, and sediment is discharged from the bottom of solid-liquid separator;
(2) supernatant that sub-argument goes out carries out alcoholysis with ethanol, and the concentration of the ethanol is 50%, and ethanol consumption is supernatant
30%, glycolysis temperature is 40 DEG C, and the alcoholysis time be 0.5h, with ethanol can make partly the silanol that not readily dissolves be dissolved into ethanol
In, to adjust methane-siliconic acid sodium content;Bottom sediment carries out alkaline hydrolysis with alkali lye, and the alkali lye is sodium hydroxide or hydroxide
Potassium, the mass fraction of alkali lye is 32%, and dosage is the 20% of sediment, and the alkaline hydrolysis time is 2h, and it is 7.5 to keep final pH, uses alkali
The high-boiling components contained in bottom precipitation can fully be dissolved;
(3) final product of alcoholysis and alkaline hydrolysis is fully incorporated sedimentation basin in step (2), is carried out with 12% Klorvess Liquid
Washing, obtains final dilution and dry slag, dry slag is dehydrated, stand-by;
(4) cement mortar is prepared together with above-mentioned dry slag and cement and sand, wherein, dry slag 8%, cement 28%, surplus
For sand, after dry-mixed, then 1.3% dilution is mixed, add water and be prepared into cement mortar for building;
(5) above-mentioned dilution is concentrated into water content as 68%, mix with organic solvent, the organic solvent for chloroform or
Phenol, its dosage are the 3% of dilution, and organic solvent can promote the progress of reaction, add 48% fat under agitation
Acid is reacted, and the aliphatic acid is polyunsaturated fatty acid, can strengthen the anti-of final product using polyunsaturated fatty acid
Water effect, about 50 DEG C of reaction temperature, the reactant that finishes will be reacted and collected, added water on demand and be configured to construction material and prevent
Aqua.
Embodiment 2:A kind of recoverying and utilizing method of organosilicon slag slurry, comprises the following steps:
(1) low-boiling-point substance of addition 35.5% is hydrolyzed in organosilicon slag slurry, and the low-boiling-point substance is chloromethanes, tetramethyl
Any one in silicon or trichlorosilane or two or more any combination, temperature control uses stirring at low speed at 46 DEG C during hydrolysis
Machine 25r/min stirring hydrolysis 5h, carry out separation of solid and liquid with solid-liquid separator by the product after hydrolysis, obtain supernatant and precipitation
Thing, supernatant are flowed out from the upper end of solid-liquid separator, and sediment is discharged from the bottom of solid-liquid separator;
(2) supernatant that sub-argument goes out carries out alcoholysis with ethanol, and the concentration of the ethanol is 57.5%, and ethanol consumption is supernatant
The 35% of liquid, glycolysis temperature are 42.5 DEG C, and the alcoholysis time is 0.75h, and the silanol that can not readily dissolve part with ethanol dissolves
Into ethanol, to adjust methane-siliconic acid sodium content;Bottom sediment carries out alkaline hydrolysis with alkali lye, and the alkali lye is sodium hydroxide or hydrogen
Potassium oxide, the mass fraction of alkali lye is 36%, and dosage is the 30% of sediment, and the alkaline hydrolysis time is 2.5h, and holding final pH is
7.7, the high-boiling components contained in bottom precipitation can fully be dissolved with alkali;
(3) final product of alcoholysis and alkaline hydrolysis is fully incorporated sedimentation basin in step (2), and the Klorvess Liquid with 13.5% enters
Water-filling is washed, and obtains final dilution and dry slag, and dry slag is dehydrated, stand-by;
(4) cement mortar is prepared together with above-mentioned dry slag and cement and sand, wherein, dry slag 10.5%, cement 30% is remaining
Measure as sand, after dry-mixed, then mix 1.9% dilution, add water and be prepared into cement mortar for building;
(5) above-mentioned dilution is concentrated into water content as 69%, mix with organic solvent, the organic solvent for chloroform or
Phenol, its dosage are the 6.5% of dilution, and organic solvent can promote the progress of reaction, add 53% fat under agitation
Fat acid is reacted, and the aliphatic acid is polyunsaturated fatty acid, can strengthen final product using polyunsaturated fatty acid
Waterproof effect, about 70 DEG C of reaction temperature, the reactant that reaction finishes is collected, add water on demand and be configured to construction material
Waterproofing agent.
Embodiment 3:A kind of recoverying and utilizing method of organosilicon slag slurry, comprises the following steps:
(1) low-boiling-point substance of addition 48% is hydrolyzed in organosilicon slag slurry, and the low-boiling-point substance is chloromethanes, tetramethylsilane
Or any one in trichlorosilane or two or more any combination, temperature control uses low-speed mixer at 47 DEG C during hydrolysis
30r/min stirring hydrolysis 7h, carry out separation of solid and liquid with solid-liquid separator by the product after hydrolysis, obtain supernatant and sediment,
Supernatant is flowed out from the upper end of solid-liquid separator, and sediment is discharged from the bottom of solid-liquid separator;
(2) supernatant that sub-argument goes out carries out alcoholysis with ethanol, and the concentration of the ethanol is 65%, and ethanol consumption is supernatant
40%, glycolysis temperature is 45 DEG C, and the alcoholysis time be 1h, with ethanol can make partly the silanol that not readily dissolves be dissolved into ethanol
In, to adjust methane-siliconic acid sodium content;Bottom sediment carries out alkaline hydrolysis with alkali lye, and the alkali lye is sodium hydroxide or hydroxide
Potassium, the mass fraction of alkali lye is 40%, and dosage is the 40% of sediment, and the alkaline hydrolysis time is 3h, and it is 8.0 to keep final pH, uses alkali
The high-boiling components contained in bottom precipitation can fully be dissolved;
(3) final product of alcoholysis and alkaline hydrolysis is fully incorporated sedimentation basin in step (2), is carried out with 15% Klorvess Liquid
Washing, obtains final dilution and dry slag, dry slag is dehydrated, stand-by;
(4) cement mortar is prepared together with above-mentioned dry slag and cement and sand, wherein, dry slag 15%, cement 32%, surplus
For sand, after dry-mixed, then 2.5% dilution is mixed, add water and be prepared into cement mortar for building;
(5) above-mentioned dilution is concentrated into water content as 70%, mix with organic solvent, the organic solvent for chloroform or
Phenol, its dosage are the 10% of dilution, and organic solvent can promote the progress of reaction, add 58% fat under agitation
Acid is reacted, and the aliphatic acid is polyunsaturated fatty acid, can strengthen the anti-of final product using polyunsaturated fatty acid
Water effect, about 90 DEG C of reaction temperature, the reactant that finishes will be reacted and collected, added water on demand and be configured to construction material and prevent
Aqua.
The organosilicon slag slurry recoverying and utilizing method simple possible of the present invention, the dry slag after hydrolysis can be used to prepare cement bonded sand
Slurry, product prevent from staiing with good hydrophobicity;Construction material waterproofing agent is made in dilution liquid energy, through waterproof of the present invention
The material of agent processing has good gas permeability, there is certain corrosion resistance, extends Building life cycle;Realize the abundant of waste
Recycle, reduce the pollution to environment, meet strategy of sustainable development requirement.
Finally it should be noted that:The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those within the art that:It still may be used
To be modified to the technical scheme described in previous embodiment, or equivalent substitution is carried out to which part technical characteristic;And
These modifications are replaced, and the essence of appropriate technical solution is departed from the spirit and model of technical scheme of the embodiment of the present invention
Enclose.