CN106634149A - Preparation method of gas-phase silicon dioxide for delustering coating - Google Patents
Preparation method of gas-phase silicon dioxide for delustering coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/69—Particle size larger than 1000 nm
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
- C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention relates to the field of the preparation of silicon dioxide, and discloses a preparation method of gas-phase silicon dioxide for a delustering coating. The preparation method comprises the following steps of 1), the preparation of silane; 2), the synthesis of gas-phase silicon dioxide; 3), the preparation of the gas-phase silicon dioxide for the delustering coating: first replacing air in a reaction kettle by using nitrogen, then conveying the gas-phase silicon dioxide made in the step 2) into the reaction kettle, meanwhile, introducing ammonia water into the reaction kettle, heating an obtained mixture, and then carrying out heat preservation, so as to obtain a semi-finished product after the ammonia water in the reaction kettle is subjected to evaporation drying; sorting the semi-finished product, then smashing, sorting a smashed material, then carrying out solid-gas separation on the material of which the particle size is in a range of 1 to 2 microns, so that the delustering gas-phase silicon dioxide is made subsequently. The gas-phase silicon dioxide made by the method provided by the invention is good in delustering performance and excellent in transparency, difficultly generates sediment, and further, has an outstanding antibacterial function. In addition, according to the method provided by the invention, the emission amount of harmful substances is small in a production process; the pollution to an environment is little.
Description
Technical field
The present invention relates to silica preparation field, more particularly to a kind of preparation side of antiglossing pigment aerosil
Method.
Background technology
The material that Coating Matting agent can make coating surface gloss and substantially reduce is referred to as Coating Matting agent, its consumption it is maximum be
Ultra tiny synthetic silica, next to that micronizing wax, aluminium, calcium, magnesium, zinc stearate consumption it is less.Disappearing with regard to film
Light principle, it is considered that first form small concavo-convex on the surface of film, the surface forms diffusing reflection to incident ray.Work as film
When being dried, due to the volatilization of solvent, surface is constantly shunk, and is made to be uniformly distributed duller particle therein and is formed atomic little on surface
It is concavo-convex.
Coating Matting agent should possess following characteristics：It is easily dispersed；Extinction performance is good, and low addition can just be produced and disappeared by force
Optical property；Transparency interference to film is little；Mechanical property and chemical property on film affects little；Suspend in liquid coating
Property it is good, can be long time stored, hard precipitation will not be produced；Little is affected on Gel-coating film spraying；Chemical inertness is high.
Micron silica delustering agent possesses above feature, thus consumption is most in coating.Its chemical purity is high, no
Water, various organic solvents and general acid, alkali are dissolved in, are only reacted with concentrated base and hydrofluoric acid, chemical inertness is high.Its refractive index is
1.46, it is close to the refractive index 1.4～1.5 of various coating resins, thus the transparency is good.With the silica delustring of Lasaxing Oilfield
Agent will not produce hard precipitation in storage process in solvent based coating.Due to being porous material, low addition just can be produced
The strong extinction of life.
Micron silica delustering agent has three types, is the amorphous porous mass of X-ray.One is heavy for micron order
Shallow lake hydrated SiO 2, precursor is piled up in chain.It is to use most one kind both at home and abroad, and price is low, because granularity is little,
Large usage quantity, the transparency is poor, is only applicable to low grade and the middle-grade coating of fraction, and foreign brand name is with Evonik Degussa Corp.
The ACEMATT＆reg of (EVONIK Degussa)；OK series mass is best, it is easy to disperse, and has Lasaxing Oilfield, and it is hard heavy to be not likely to produce
Form sediment.
Another kind is micron silica aeroge, and its precursor forms three-dimensional space net structure, and pore volume is general
More than 1.5mL/g.The country has produced, due to using micron and submicron order grading plant, narrow particle size distribution, and extinction and thoroughly
Bright property is suitable with veriety with foreign countries.Using Lasaxing Oilfield technique, long-time is placed will not produce hard precipitation.External mainstream product
For W. R. Grace ＆ Co (GRACE DAVISON) SYLOID＆reg；C series delustering agents；INEOS companies Gasil and HP series delustrings
Agent.
The third is aerosil delustering agent, with the most work that Evonik Degussa Corp. (EVONIK Degussa) produces
Name, ACEMATT＆reg；TS100 and TT600.Its extinction performance is good, excellent transparency, but is easy to produce precipitation.
The content of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of preparation side of antiglossing pigment aerosil
Method.Aerosil extinction performance is good obtained in the inventive method, excellent transparency, and is not likely to produce precipitation.And produced
Discharge of poisonous waste amount is few in journey, and environmental pollution is little.
The present invention concrete technical scheme be：A kind of preparation method of antiglossing pigment aerosil, including it is following
Step：
1) silane synthesis；
2) aerosil synthesis；
3) preparation of antiglossing pigment aerosil：
First with the air in nitrogen displacement reactor, then by step 2) obtained in aerosil be delivered to reactor,
Simultaneously by quality for aerosil 4-6%, concentration be passed through reactor for the ammoniacal liquor of 24-26wt%, be heated to 175-185
It is incubated after DEG C, in question response kettle after ammoniacal liquor evaporation drying, obtains semi-finished product；Semi-finished product are pumped into 1# semi-finished product storage tanks, it is sorted
Crushed after device sorting, the material after crushing enters 2# semi-finished product storage tanks, after sorted device sorting, by particle diameter in 1-2 microns
Material outside scope is again introduced into returning to 2# semi-finished product storage tanks after pulverizer is crushed；To particle diameter 1-2 micrometer ranges material Jing
After crossing solid and gas separation, delustring aerosil is obtained.
In step 3) in, chemical reaction, the above-mentioned works of aerosil Jing are not related between aerosil and ammoniacal liquor
Particle diameter rises to 1～2 μm by 90nm after skill process, becomes delustring aerosil.Gas phase dioxy obtained in the inventive method
SiClx extinction performance is good, excellent transparency, and is not likely to produce precipitation.
Preferably, step 1) silane synthetic method be：
Metallic silicon, HCl are added and is reacted into reactor, hydrogen is passed through during the course of the reaction, after reaction terminates, will
Gas in reactor is washed by filter and removes the metallic silicon not reacted, gas through heat exchanger cooling point after dedusting
From rear, it is divided into three parts：Byproduct hydrogen gas, intermediate SiHCl3、SiCl4And solid and gas separates waste gas；
Wherein, the byproduct hydrogen gas are back to respectively silane synthesis and follow-up aerosil synthesis；The centre
Body SiHCl3、SiCl4Jing separateds, deliver to respectively storage area and keep in；
The solid and gas that refrigerated separation is produced separates waste gas, uncooled waste gas, SiHCl that separated is produced3、SiCl4And
CH3SiCl3The storage tank breathing waste gas that storage tank Big and Small Breath is produced；What filter was produced unloads the distillation that dirt waste water, separated are produced
Raffinate is admitted to waste gas, waste liquid and removes the evil workshop section.
Preferably, step 2) aerosil synthetic method is：
By step 1) SiCl after separated4、SiHCl3Or the CH for separately adding3SiCl3Heated into promoting the circulation of qi with steam
Change, fully react with the hydrogen, excess air for adding, form aerosil and byproduct HCl；
Wherein, in course of reaction hydrogen portion derive from step 1) byproduct hydrogen gas；After reaction terminates, gas phase two will be contained
The gas of silica is condensed by knockouts, then by the isolated aerosil of solid and gas；Then to aerosil
Depickling process is carried out with steam, electrothermal drying, cooling is carried out after depickling again；Finally bulk density adjustment is carried out using volume machine；
Step 2) in solid and gas separation, depickling, be dried produce mix waste gas be admitted to HCl recovery workshop section.
Preferably, in step 2) described in HCl recovery workshop section in, step 2) in solid and gas separate, depickling and be dried produce
Mix waste gas first pass through filter washing except deentrainment a small amount of SiO2, after dedusting in gas HCl Jing concentration 21wt% hydrochloric acid
Solution three-level water absorption, forms the hydrochloric acid solution that concentration is 31wt%；The hydrochloric acid solution dress of the 31wt% of partially recycled gained
Enter storage tank export trade, remaining hydrochloric acid solution carries out de- analysis, the HCl for obtaining is used for step 1 Jing after the dehydration of the 98wt% concentrated sulfuric acids) silane
Synthesis；The concentration of hydrochloric acid solution of 31wt% is dropped back to 21wt% after de- analysis, and fully recovering absorbs in HCl；
It is net that the mix waste gas washed after dedusting, three-level water system absorb through filter sequentially pass through again washing, two grades of alkali cleanings
After change, the high aiutage high altitude discharges of Jing 25m, it is ensured that HCl concentration of emissions are not higher than 5ppm Jing after absorption cleaning；Hydrochloric acid tank size
Storage tank breathing the washing with water of waste gas that breathing is produced, is re-fed into being discharged after caustic wash tower alkali cleaning purification；
Waste water after wherein above-mentioned washing is used as the water source of above-mentioned filter washing.
Preferably, after the described 98wt% concentrated sulfuric acids are dried to the HCl that de- analysis is obtained, obtaining the sulphur of 90wt%
Acid, after being deployed into the dilute sulfuric acid of 20wt%, uses as the raw material of inorganic flocculating agent：By sodium metasilicate and the sulfuric acid of 20wt%
After hybrid reaction, aluminum sulfate is added, make aluminium salt inorganic flocculating agent.
In the preferred version of the present invention, silane synthesis and silica synthesis adopt Homemade method, using said method
Homemade silane and silica, in process of production can the various accessory substances of effective recycling, and be greatly decreased harmful
The discharge capacity of material, environmental pollution is little, meets the theory of environmental protection.
Preferably, step 3) obtained in delustring aerosil also through modification：
A) weigh delustring aerosil and be configured to the suspension that concentration is 8-12wt%, separately prepare respectively
Concentration is silver nitrate solution, magnesium nitrate solution and the copper nitrate solution of 8-12wt%；Successively by silver nitrate solution, magnesium nitrate solution
It is added drop-wise in suspension and is uniformly dispersed with copper nitrate solution, obtains mixed liquor A；Wherein silver nitrate solution, magnesium nitrate solution and
The consumption of copper nitrate solution is respectively 8-12%, 5-7%, 3-5% of suspension vol.
B) by tetraethyl orthosilicate, absolute ethyl alcohol and water by volume 1:4-6:2-3 mixes, and after stirring, is with concentration
It is 4-6 that the salpeter solution of 0.1mol/L adjusts pH, obtains mixed liquid B；Mixed liquor A is transferred in 50-55 DEG C of water-bath, in stirring
Under the conditions of mixed liquid B is added drop-wise in mixed liquor A, wherein the quality of mixed liquid B for mixed liquor A 4-8%.
C after) mixed liquid B is dripped, by product at 60-65 DEG C still aging 1-3h；Obtain improved silica
Colloidal sol；Modified silicon dioxide sol is dried at 100-110 DEG C, powder is then ground to, roasting 1-2h takes at 400-600 DEG C
Go out, modified delustring aerosil is obtained after regrinding.
Through the modified delustring aerosil that above-mentioned modification is obtained, with outstanding antibacterial functions.Current
In some antiglossing pigments, it will usually which adding some antiseptics makes coating have certain antibiotic property.But In the view of at present, generally
There is following defect：1st, antiseptic bad dispersibility in coating；2nd, antiseptic is high to place environmental requirement, and antibacterial is lived in coating
Property reduce, antibacterial effect cannot give full play to；3rd, antiseptic stability in coating it is poor, volatile, be lost in, Durability of antimicrobial effect
Difference；4th, it is harmful after the volatilization of part antiseptic.
The present invention first mixes the suspension of delustring aerosil with the solution containing silver ion, magnesium ion, copper ion
Close uniform, obtain mixed liquor A, then mixed liquid B is added drop-wise into mixed liquor A and is reacted, sol system is formed after ageing, be dried
Afterwards through high-temperature roasting, the removal of impurity is gone, the flatting silica for being loaded with three metal ion species is obtained.Obtained silica into
The dioxy for being coated with metal/metal ion that product are formed based on delustring aerosil, later stage by sol-gel process
Supplemented by SiClx, both combine.
In said method, by approach such as a series of physical absorption and ion-exchange reactions, there is antibacterial energy by three kinds
The metal or metal ion of power and micro- magnetic field permanent magnet performance is loaded on silica, with following technique effect：
1st, because delustring aerosil has preferably dispersiveness in coating, therefore antiseptic dispersiveness is solved not
Good technical problem.
2nd, because metal or metal ion possess silica as carrier, load fastness is good, and stability is obtained in coating
To raising, not easily run off, solve antiseptic and stablize poor, volatile, loss, the technical problem of Durability of antimicrobial effect difference.
3rd, metal or metal ion antimicrobial component are nontoxic to human body.
4th, above-mentioned metal or metal ion obtain the protection of carrier, low to environmental requirements such as humitures, the antibacterial in coating
Activity is good.And above-mentioned metal or metal ion coupled ion antibacterial mechanisms and micro- magnetoelectricity field technology principle, on the one hand can interfere with
The synthesis of cell membrane and destruction cell membrane, cell loses the protective effect to osmotic pressure, finally makes bacterial death.The opposing party
Face can above-mentioned metal or metal ion suppress the synthesis of protein by exchange of particles method, make bacterial death.The present invention passes through
Micro- magnetic field strengthens the ionization activity and intensity of metal ion, therefore with more outstanding antibacterial effect.
Preferably, step B) in, the drop rate of mixed liquid B is 2-4mL/min.
Preferably, step 3) in, the specific surface area of the delustring aerosil for finally obtaining is 150 ± 20m2/g。
It is compared with the prior art, the invention has the beneficial effects as follows：Aerosil extinction obtained in the inventive method
Good, the excellent transparency of energy, is not likely to produce precipitation and with outstanding antibacterial functions.In addition the inventive method is harmful in process of production
Matter emissions are few, and environmental pollution is little.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of antiglossing pigment aerosil, comprises the following steps：
1) using conventional method synthesizing silane SiHCl3、SiCl4。
2) aerosil synthesis：With SiHCl3、SiCl4For primary raw material, gas phase titanium dioxide is synthesized using conventional method
Silicon.
3) preparation of antiglossing pigment aerosil：
First with the air in nitrogen displacement reactor, then by step 2) obtained in aerosil be delivered to reactor,
Simultaneously by quality for aerosil 5%, concentration be passed through reactor for the ammoniacal liquor of 25wt%, be incubated after being heated to 180 DEG C,
In question response kettle after ammoniacal liquor evaporation drying, semi-finished product are obtained；Semi-finished product are pumped into 1# semi-finished product storage tanks, sorted device sorting is laggard
Row is crushed, and the material after crushing enters 2# semi-finished product storage tanks, after sorted device sorting, by thing of the particle diameter outside 1-2 micrometer ranges
Material is again introduced into returning to 2# semi-finished product storage tanks after pulverizer is crushed；To particle diameter 1-2 micrometer ranges material Jing sack cleaners
Solid and gas enters finished product storage tank after separating, and flatting silica is obtained Jing after vacuum packing machine packaging can warehouse-in.Produce for batch,
Often produce and need to purge reactor after a batch, cleaned.Obtained aerosil specific surface area be 150 ±
20m2/g
Embodiment 2
A kind of preparation method of antiglossing pigment aerosil, comprises the following steps：
1) silane synthesis：
Metallic silicon, HCl are added and is reacted into reactor, hydrogen is passed through during the course of the reaction, after reaction terminates, will
Gas in reactor is washed by filter and removes the metallic silicon not reacted, gas through heat exchanger cooling point after dedusting
From rear, it is divided into three parts：Byproduct hydrogen gas, intermediate SiHCl3、SiCl4And solid and gas separates waste gas.
Wherein, the byproduct hydrogen gas are back to respectively silane synthesis and follow-up aerosil synthesis；The centre
Body SiHCl3、SiCl4Jing separateds, deliver to respectively storage area and keep in.
The solid and gas that refrigerated separation is produced separates waste gas, uncooled waste gas, SiHCl that separated is produced3、SiCl4And
CH3SiCl3The storage tank breathing waste gas that storage tank Big and Small Breath is produced；What filter was produced unloads the distillation that dirt waste water, separated are produced
Raffinate is admitted to waste gas, waste liquid and removes the evil workshop section.
Step 1) reaction principle be：
Main reaction：
Si+3HCl→SiHCl3+H2
Si+4HCl→SiCl4+2H2
There is side reaction in impurity：
2Al+6HCl→2AlCl3+3H2
2Fe+6HCl→2FeCl3+3H2
2) aerosil synthesis：
By step 1) SiCl after separated4、SiHCl3Or the CH for separately adding3SiCl3Heated into promoting the circulation of qi with steam
Change, fully react with the hydrogen, excess air for adding, form aerosil and byproduct HCl.
Wherein, in course of reaction hydrogen portion derive from step 1) byproduct hydrogen gas；After reaction terminates, gas phase two will be contained
The gas of silica is condensed by knockouts, then by the isolated aerosil of solid and gas；Then to aerosil
Depickling process is carried out with steam, electrothermal drying, cooling is carried out after depickling again；Finally bulk density adjustment is carried out using volume machine；
Step 2) in solid and gas separation, depickling, be dried produce mix waste gas be admitted to HCl recovery workshop section.
In described HCl recovery workshop section, step 2) in solid and gas separate, depickling and be dried the mix waste gas elder generation Jing for producing
Filter washing is except a small amount of SiO of deentrainment2, the hydrochloric acid solution three-level washing of HCl Jing concentration 21wt% is inhaled in gas after dedusting
Receive, form the hydrochloric acid solution that concentration is 31wt%；The hydrochloric acid solution of the 31wt% of partially recycled gained loads storage tank export trade, remaining
Hydrochloric acid solution carries out de- analysis, and the HCl for obtaining is used for step 1 Jing after the dehydration of the 98wt% concentrated sulfuric acids) silane synthesis；After de- analysis
The concentration of hydrochloric acid solution of 31wt% is dropped back to 21wt%, and fully recovering absorbs in HCl.
It is net that the mix waste gas washed after dedusting, three-level water system absorb through filter sequentially pass through again washing, two grades of alkali cleanings
After change, the high aiutage high altitude discharges of Jing 25m, it is ensured that HCl concentration of emissions are not higher than 5ppm Jing after absorption cleaning；Hydrochloric acid tank size
Storage tank breathing the washing with water of waste gas that breathing is produced, is re-fed into being discharged after caustic wash tower alkali cleaning purification.
Waste water after wherein above-mentioned washing is used as the water source of above-mentioned filter washing.The described 98wt% concentrated sulfuric acids are to de- analysis
After the HCl for obtaining is dried, the sulfuric acid of 90wt% is obtained, after being deployed into the dilute sulfuric acid of 20wt%, as inorganic flocculation
The raw material of agent is used：After the sulfuric acid hybrid reaction of sodium metasilicate and 20wt%, aluminum sulfate is added, make aluminium salt inorganic flocculating agent.
Step 2) reaction principle be：
Main reaction：
SiHCl3+H2+O2→SiO2+3HCl
SiCl4+2H2+O2→SiO2+4HCl
CH3SiCl3+2O2→SiO2+3HCl+CO2
Side reaction：
4HCl+O2→2Cl2+2H2O
2H2+O2→2H2O
Step 2) in HCl recovery workshop section exhaust-gas treatment principle be：
Cl2+2NaOH→NaClO+NaCl+H2O
HCl+NaOH→NaCl+H2O
3) preparation of antiglossing pigment aerosil：
First with the air in nitrogen displacement reactor, then by step 2) obtained in aerosil be delivered to reactor,
Simultaneously by quality for aerosil 4%, concentration be passed through reactor for the ammoniacal liquor of 24wt%, be incubated after being heated to 175 DEG C,
In question response kettle after ammoniacal liquor evaporation drying, semi-finished product are obtained；Semi-finished product are pumped into 1# semi-finished product storage tanks, sorted device sorting is laggard
Row is crushed, and the material after crushing enters 2# semi-finished product storage tanks, after sorted device sorting, by thing of the particle diameter outside 1-2 micrometer ranges
Material is again introduced into returning to 2# semi-finished product storage tanks after pulverizer is crushed；Material of the particle diameter in 1-2 micrometer ranges is separated through solid and gas
Afterwards, the specific surface area that delustring aerosil is obtained is 150 ± 20m2/g。
Embodiment 3
1) silane synthesis：
Metallic silicon, HCl are added and is reacted into reactor, hydrogen is passed through during the course of the reaction, after reaction terminates, will
Gas in reactor is washed by filter and removes the metallic silicon not reacted, gas through heat exchanger cooling point after dedusting
From rear, it is divided into three parts：Byproduct hydrogen gas, intermediate SiHCl3、SiCl4And solid and gas separates waste gas.
Wherein, the byproduct hydrogen gas are back to respectively silane synthesis and follow-up aerosil synthesis；The centre
Body SiHCl3、SiCl4Jing separateds, deliver to respectively storage area and keep in.
The solid and gas that refrigerated separation is produced separates waste gas, uncooled waste gas, SiHCl that separated is produced3、SiCl4And
CH3SiCl3The storage tank breathing waste gas that storage tank Big and Small Breath is produced；What filter was produced unloads the distillation that dirt waste water, separated are produced
Raffinate is admitted to waste gas, waste liquid and removes the evil workshop section.
Step 1) reaction principle be：
Main reaction：
Si+3HCl→SiHCl3+H2
Si+4HCl→SiCl4+2H2
There is side reaction in impurity：
2Al+6HCl→2AlCl3+3H2
2Fe+6HCl→2FeCl3+3H2
By step 1) SiCl after separated4、SiHCl3Or the CH for separately adding3SiCl3Heated into promoting the circulation of qi with steam
Change, fully react with the hydrogen, excess air for adding, form aerosil and byproduct HCl.
Wherein, in course of reaction hydrogen portion derive from step 1) byproduct hydrogen gas；After reaction terminates, gas phase two will be contained
The gas of silica is condensed by knockouts, then by the isolated aerosil of solid and gas；Then to aerosil
Depickling process is carried out with steam, electrothermal drying, cooling is carried out after depickling again；Finally bulk density adjustment is carried out using volume machine；
Step 2) in solid and gas separation, depickling, be dried produce mix waste gas be admitted to HCl recovery workshop section.
In described HCl recovery workshop section, step 2) in solid and gas separate, depickling and be dried the mix waste gas elder generation Jing for producing
Filter washing is except a small amount of SiO of deentrainment2, the hydrochloric acid solution three-level washing of HCl Jing concentration 21wt% is inhaled in gas after dedusting
Receive, form the hydrochloric acid solution that concentration is 31wt%；The hydrochloric acid solution of the 31wt% of partially recycled gained loads storage tank export trade, remaining
Hydrochloric acid solution carries out de- analysis, and the HCl for obtaining is used for step 1 Jing after the dehydration of the 98wt% concentrated sulfuric acids) silane synthesis；After de- analysis
The concentration of hydrochloric acid solution of 31wt% is dropped back to 21wt%, and fully recovering absorbs in HCl.
It is net that the mix waste gas washed after dedusting, three-level water system absorb through filter sequentially pass through again washing, two grades of alkali cleanings
After change, the high aiutage high altitude discharges of Jing 25m, it is ensured that HCl concentration of emissions are not higher than 5ppm Jing after absorption cleaning；Hydrochloric acid tank size
Storage tank breathing the washing with water of waste gas that breathing is produced, is re-fed into being discharged after caustic wash tower alkali cleaning purification.
Waste water after wherein above-mentioned washing is used as the water source of above-mentioned filter washing.The described 98wt% concentrated sulfuric acids are to de- analysis
After the HCl for obtaining is dried, the sulfuric acid of 90wt% is obtained, after being deployed into the dilute sulfuric acid of 20wt%, as inorganic flocculation
The raw material of agent is used：After the sulfuric acid hybrid reaction of sodium metasilicate and 20wt%, aluminum sulfate is added, make aluminium salt inorganic flocculating agent.
Step 2) reaction principle be：
Main reaction：
SiHCl3+H2+O2→SiO2+3HCl
SiCl4+2H2+O2→SiO2+4HCl
CH3SiCl3+2O2→SiO2+3HCl+CO2
Side reaction：
4HCl+O2→2Cl2+2H2O
2H2+O2→2H2O
Step 2) in HCl recovery workshop section exhaust-gas treatment principle be：
Cl2+2NaOH→NaClO+NaCl+H2O
HCl+NaOH→NaCl+H2O
3) preparation of antiglossing pigment aerosil：
First with the air in nitrogen displacement reactor, then by step 2) obtained in aerosil be delivered to reactor,
Simultaneously by quality for aerosil 6%, concentration be passed through reactor for the ammoniacal liquor of 26wt%, be incubated after being heated to 185 DEG C,
In question response kettle after ammoniacal liquor evaporation drying, semi-finished product are obtained；Semi-finished product are pumped into 1# semi-finished product storage tanks, sorted device sorting is laggard
Row is crushed, and the material after crushing enters 2# semi-finished product storage tanks, after sorted device sorting, by thing of the particle diameter outside 1-2 micrometer ranges
Material is again introduced into returning to 2# semi-finished product storage tanks after pulverizer is crushed；Material of the particle diameter in 1-2 micrometer ranges is separated through solid and gas
Afterwards, delustring aerosil is obtained.
4) modification：
A) weigh delustring aerosil and be configured to the suspension that concentration is 10wt%, separately prepare respectively dense
Spend silver nitrate solution for 10wt%, magnesium nitrate solution and copper nitrate solution；Successively by silver nitrate solution, magnesium nitrate solution and nitre
Sour copper solution is added drop-wise in suspension and is uniformly dispersed, and obtains mixed liquor A；Wherein silver nitrate solution, magnesium nitrate solution and nitric acid
The consumption of copper solution is respectively 10%, 6%, the 4% of suspension vol.
B) by tetraethyl orthosilicate, absolute ethyl alcohol and water by volume 1:5:2.5 mixing, after stirring, be with concentration
It is 5 that the salpeter solution of 0.1mol/L adjusts pH, obtains mixed liquid B；Mixed liquor A is transferred in 52 DEG C of water-baths, in stirring condition
Lower mixed liquid B to be added drop-wise in mixed liquor A with the speed of 3mL/min, wherein the quality of mixed liquid B is the 6% of mixed liquor A.
C after) mixed liquid B is dripped, by product at 62 DEG C still aging 2h；Obtain modified silicon dioxide sol；
Modified silicon dioxide sol is dried at 105 DEG C, powder is then ground to, roasting 1.5h takes out at 500 DEG C, after regrinding
Modified delustring aerosil is obtained, specific surface area is 150 ± 20m2/g。
Embodiment 4
1) silane synthesis：
Metallic silicon, HCl are added and is reacted into reactor, hydrogen is passed through during the course of the reaction, after reaction terminates, will
Gas in reactor is washed by filter and removes the metallic silicon not reacted, gas through heat exchanger cooling point after dedusting
From rear, it is divided into three parts：Byproduct hydrogen gas, intermediate SiHCl3、SiCl4And solid and gas separates waste gas.
Wherein, the byproduct hydrogen gas are back to respectively silane synthesis and follow-up aerosil synthesis；The centre
Body SiHCl3、SiCl4Jing separateds, deliver to respectively storage area and keep in.
The solid and gas that refrigerated separation is produced separates waste gas, uncooled waste gas, SiHCl that separated is produced3、SiCl4And
CH3SiCl3The storage tank breathing waste gas that storage tank Big and Small Breath is produced；What filter was produced unloads the distillation that dirt waste water, separated are produced
Raffinate is admitted to waste gas, waste liquid and removes the evil workshop section.
Step 1) reaction principle be：
Main reaction：
Si+3HCl→SiHCl3+H2
Si+4HCl→SiCl4+2H2
There is side reaction in impurity：
2Al+6HCl→2AlCl3+3H2
2Fe+6HCl→2FeCl3+3H2
By step 1) SiCl after separated4、SiHCl3Or the CH for separately adding3SiCl3Heated into promoting the circulation of qi with steam
Change, fully react with the hydrogen, excess air for adding, form aerosil and byproduct HCl.
Wherein, in course of reaction hydrogen portion derive from step 1) byproduct hydrogen gas；After reaction terminates, gas phase two will be contained
The gas of silica is condensed by knockouts, then by the isolated aerosil of solid and gas；Then to aerosil
Depickling process is carried out with steam, electrothermal drying, cooling is carried out after depickling again；Finally bulk density adjustment is carried out using volume machine；
Step 2) in solid and gas separation, depickling, be dried produce mix waste gas be admitted to HCl recovery workshop section.
In described HCl recovery workshop section, step 2) in solid and gas separate, depickling and be dried the mix waste gas elder generation Jing for producing
Filter washing is except a small amount of SiO of deentrainment2, the hydrochloric acid solution three-level washing of HCl Jing concentration 21wt% is inhaled in gas after dedusting
Receive, form the hydrochloric acid solution that concentration is 31wt%；The hydrochloric acid solution of the 31wt% of partially recycled gained loads storage tank export trade, remaining
Hydrochloric acid solution carries out de- analysis, and the HCl for obtaining is used for step 1 Jing after the dehydration of the 98wt% concentrated sulfuric acids) silane synthesis；After de- analysis
The concentration of hydrochloric acid solution of 31wt% is dropped back to 21wt%, and fully recovering absorbs in HCl.
It is net that the mix waste gas washed after dedusting, three-level water system absorb through filter sequentially pass through again washing, two grades of alkali cleanings
After change, the high aiutage high altitude discharges of Jing 25m, it is ensured that HCl concentration of emissions are not higher than 5ppm Jing after absorption cleaning；Hydrochloric acid tank size
Storage tank breathing the washing with water of waste gas that breathing is produced, is re-fed into being discharged after caustic wash tower alkali cleaning purification.
Waste water after wherein above-mentioned washing is used as the water source of above-mentioned filter washing.The described 98wt% concentrated sulfuric acids are to de- analysis
After the HCl for obtaining is dried, the sulfuric acid of 90wt% is obtained, after being deployed into the dilute sulfuric acid of 20wt%, as inorganic flocculation
The raw material of agent is used：After the sulfuric acid hybrid reaction of sodium metasilicate and 20wt%, aluminum sulfate is added, make aluminium salt inorganic flocculating agent.
Step 2) reaction principle be：
Main reaction：
SiHCl3+H2+O2→SiO2+3HCl
SiCl4+2H2+O2→SiO2+4HCl
CH3SiCl3+2O2→SiO2+3HCl+CO2
Side reaction：
4HCl+O2→2Cl2+2H2O
2H2+O2→2H2O
Step 2) in HCl recovery workshop section exhaust-gas treatment principle be：
Cl2+2NaOH→NaClO+NaCl+H2O
HCl+NaOH→NaCl+H2O
3) preparation of antiglossing pigment aerosil：
First with the air in nitrogen displacement reactor, then by step 2) obtained in aerosil be delivered to reactor,
Simultaneously by quality for aerosil 5%, concentration be passed through reactor for the ammoniacal liquor of 25wt%, be incubated after being heated to 180 DEG C,
In question response kettle after ammoniacal liquor evaporation drying, semi-finished product are obtained；Semi-finished product are pumped into 1# semi-finished product storage tanks, sorted device sorting is laggard
Row is crushed, and the material after crushing enters 2# semi-finished product storage tanks, after sorted device sorting, by thing of the particle diameter outside 1-2 micrometer ranges
Material is again introduced into returning to 2# semi-finished product storage tanks after pulverizer is crushed；Material of the particle diameter in 1-2 micrometer ranges is separated through solid and gas
Afterwards, delustring aerosil is obtained.
4) modification：
A) weigh delustring aerosil and be configured to the suspension that concentration is 8wt%, separately prepare respectively dense
Spend silver nitrate solution for 8wt%, magnesium nitrate solution and copper nitrate solution；Successively by silver nitrate solution, magnesium nitrate solution and nitre
Sour copper solution is added drop-wise in suspension and is uniformly dispersed, and obtains mixed liquor A；Wherein silver nitrate solution, magnesium nitrate solution and nitric acid
The consumption of copper solution is respectively 8%, 5%, the 3% of suspension vol.
B) by tetraethyl orthosilicate, absolute ethyl alcohol and water by volume 1:4:2 mixing, after stirring, be with concentration
It is 4 that the salpeter solution of 0.1mol/L adjusts pH, obtains mixed liquid B；Mixed liquor A is transferred in 50 DEG C of water-baths, in stirring condition
Lower mixed liquid B to be added drop-wise in mixed liquor A with the speed of 2mL/min, wherein the quality of mixed liquid B is the 4% of mixed liquor A.
C after) mixed liquid B is dripped, by product at 60 DEG C still aging 3h；Obtain modified silicon dioxide sol；
Modified silicon dioxide sol is dried at 100 DEG C, powder is then ground to, roasting 2h takes out at 400 DEG C, after regrinding
To modified delustring aerosil, specific surface area is 150 ± 20m2/g。
Embodiment 5
1) silane synthesis：
Metallic silicon, HCl are added and is reacted into reactor, hydrogen is passed through during the course of the reaction, after reaction terminates, will
Gas in reactor is washed by filter and removes the metallic silicon not reacted, gas through heat exchanger cooling point after dedusting
From rear, it is divided into three parts：Byproduct hydrogen gas, intermediate SiHCl3、SiCl4And solid and gas separates waste gas.
Wherein, the byproduct hydrogen gas are back to respectively silane synthesis and follow-up aerosil synthesis；The centre
Body SiHCl3、SiCl4Jing separateds, deliver to respectively storage area and keep in.
The solid and gas that refrigerated separation is produced separates waste gas, uncooled waste gas, SiHCl that separated is produced3、SiCl4And
CH3SiCl3The storage tank breathing waste gas that storage tank Big and Small Breath is produced；What filter was produced unloads the distillation that dirt waste water, separated are produced
Raffinate is admitted to waste gas, waste liquid and removes the evil workshop section.
Step 1) reaction principle be：
Main reaction：
Si+3HCl→SiHCl3+H2
Si+4HCl→SiCl4+2H2
There is side reaction in impurity：
2Al+6HCl→2AlCl3+3H2
2Fe+6HCl→2FeCl3+3H2
By step 1) SiCl after separated4、SiHCl3Or the CH for separately adding3SiCl3Heated into promoting the circulation of qi with steam
Change, fully react with the hydrogen, excess air for adding, form aerosil and byproduct HCl.
Wherein, in course of reaction hydrogen portion derive from step 1) byproduct hydrogen gas；After reaction terminates, gas phase two will be contained
The gas of silica is condensed by knockouts, then by the isolated aerosil of solid and gas；Then to aerosil
Depickling process is carried out with steam, electrothermal drying, cooling is carried out after depickling again；Finally bulk density adjustment is carried out using volume machine；
Step 2) in solid and gas separation, depickling, be dried produce mix waste gas be admitted to HCl recovery workshop section.
In described HCl recovery workshop section, step 2) in solid and gas separate, depickling and be dried the mix waste gas elder generation Jing for producing
Filter washing is except a small amount of SiO of deentrainment2, the hydrochloric acid solution three-level washing of HCl Jing concentration 21wt% is inhaled in gas after dedusting
Receive, form the hydrochloric acid solution that concentration is 31wt%；The hydrochloric acid solution of the 31wt% of partially recycled gained loads storage tank export trade, remaining
Hydrochloric acid solution carries out de- analysis, and the HCl for obtaining is used for step 1 Jing after the dehydration of the 98wt% concentrated sulfuric acids) silane synthesis；After de- analysis
The concentration of hydrochloric acid solution of 31wt% is dropped back to 21wt%, and fully recovering absorbs in HCl.
It is net that the mix waste gas washed after dedusting, three-level water system absorb through filter sequentially pass through again washing, two grades of alkali cleanings
After change, the high aiutage high altitude discharges of Jing 25m, it is ensured that HCl concentration of emissions are not higher than 5ppm Jing after absorption cleaning；Hydrochloric acid tank size
Storage tank breathing the washing with water of waste gas that breathing is produced, is re-fed into being discharged after caustic wash tower alkali cleaning purification.
Waste water after wherein above-mentioned washing is used as the water source of above-mentioned filter washing.The described 98wt% concentrated sulfuric acids are to de- analysis
After the HCl for obtaining is dried, the sulfuric acid of 90wt% is obtained, after being deployed into the dilute sulfuric acid of 20wt%, as inorganic flocculation
The raw material of agent is used：After the sulfuric acid hybrid reaction of sodium metasilicate and 20wt%, aluminum sulfate is added, make aluminium salt inorganic flocculating agent.
Step 2) reaction principle be：
Main reaction：
SiHCl3+H2+O2→SiO2+3HCl
SiCl4+2H2+O2→SiO2+4HCl
CH3SiCl3+2O2→SiO2+3HCl+CO2
Side reaction：
4HCl+O2→2Cl2+2H2O
2H2+O2→2H2O
Step 2) in HCl recovery workshop section exhaust-gas treatment principle be：
Cl2+2NaOH→NaClO+NaCl+H2O
HCl+NaOH→NaCl+H2O
3) preparation of antiglossing pigment aerosil：
First with the air in nitrogen displacement reactor, then by step 2) obtained in aerosil be delivered to reactor,
Simultaneously by quality for aerosil 5%, concentration be passed through reactor for the ammoniacal liquor of 25wt%, be incubated after being heated to 180 DEG C,
In question response kettle after ammoniacal liquor evaporation drying, semi-finished product are obtained；Semi-finished product are pumped into 1# semi-finished product storage tanks, sorted device sorting is laggard
Row is crushed, and the material after crushing enters 2# semi-finished product storage tanks, after sorted device sorting, by thing of the particle diameter outside 1-2 micrometer ranges
Material is again introduced into returning to 2# semi-finished product storage tanks after pulverizer is crushed；Material of the particle diameter in 1-2 micrometer ranges is separated through solid and gas
Afterwards, delustring aerosil is obtained.
4) modification：
A) weigh delustring aerosil and be configured to the suspension that concentration is 12wt%, separately prepare respectively dense
Spend silver nitrate solution for 12wt%, magnesium nitrate solution and copper nitrate solution；Successively by silver nitrate solution, magnesium nitrate solution and nitre
Sour copper solution is added drop-wise in suspension and is uniformly dispersed, and obtains mixed liquor A；Wherein silver nitrate solution, magnesium nitrate solution and nitric acid
The consumption of copper solution is respectively 12%, 7%, the 5% of suspension vol.
B) by tetraethyl orthosilicate, absolute ethyl alcohol and water by volume 1:6:3 mixing, after stirring, be with concentration
It is 6 that the salpeter solution of 0.1mol/L adjusts pH, obtains mixed liquid B；Mixed liquor A is transferred in 55 DEG C of water-baths, in stirring condition
Lower mixed liquid B to be added drop-wise in mixed liquor A with the speed of 4mL/min, wherein the quality of mixed liquid B is the 8% of mixed liquor A.
C after) mixed liquid B is dripped, by product at 65 DEG C still aging 1h；Obtain modified silicon dioxide sol；
Modified silicon dioxide sol is dried at 110 DEG C, powder is then ground to, roasting 1h takes out at 600 DEG C, after regrinding
To modified delustring aerosil, specific surface area is 150 ± 20m2/g。
Aerosil obtained in the present invention is detected, testing result is：
1st, N2 adsorption specific surface area, m2/g(GB/T 10722-2003)：169m；
2nd, pH value (GB/T 1717-1986)：4.24；
3rd, 105 DEG C of volatile matters, % (GB/T 5211.3-1985)：1.20；
4th, burning decrement, % (GB/T 20020-2005)：2.10；
5th, chloride content, % (GB/T 20020-2005)：0.024.
Raw materials used in the present invention, equipment, unless otherwise noted, is the conventional raw material, equipment of this area；In the present invention
Method therefor, unless otherwise noted, is the conventional method of this area.
The above, is only presently preferred embodiments of the present invention, and not the present invention is imposed any restrictions, every according to the present invention
Any simple modification, change and equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (8)
1. a kind of preparation method of antiglossing pigment aerosil, it is characterised in that comprise the following steps：
1) silane synthesis；
2) aerosil synthesis；
3) preparation of antiglossing pigment aerosil：
First with the air in nitrogen displacement reactor, then by step 2) obtained in aerosil be delivered to reactor, while
By quality for aerosil 4-6%, concentration be passed through reactor for the ammoniacal liquor of 24-26wt%, after being heated to 175-185 DEG C
Insulation, in question response kettle after ammoniacal liquor evaporation drying, obtains semi-finished product；Semi-finished product are pumped into 1# semi-finished product storage tanks, sorted device point
Crushed after choosing, the material after crushing enters 2# semi-finished product storage tanks, after sorted device sorting, by particle diameter in 1-2 micrometer ranges
Outer material is again introduced into returning to 2# semi-finished product storage tanks after pulverizer is crushed；Solid is passed through in the material of 1-2 micrometer ranges to particle diameter
After gas is separated, delustring aerosil is obtained.
2. a kind of preparation method of antiglossing pigment aerosil as claimed in claim 1, it is characterised in that：Step 1)
Silane synthetic method be：
Metallic silicon, HCl are added and is reacted into reactor, hydrogen is passed through during the course of the reaction, after reaction terminates, will be reacted
Gas in device is washed by filter and removes the metallic silicon not reacted, gas through heat exchanger refrigerated separation after dedusting
Afterwards, it is divided into three parts：Byproduct hydrogen gas, intermediate SiHCl3、SiCl4And solid and gas separates waste gas；
Wherein, the byproduct hydrogen gas are back to respectively silane synthesis and follow-up aerosil synthesis；The intermediate
SiHCl3、SiCl4Jing separateds, deliver to respectively storage area and keep in；
The solid and gas that refrigerated separation is produced separates waste gas, uncooled waste gas, SiHCl that separated is produced3、SiCl4And CH3SiCl3
The storage tank breathing waste gas that storage tank Big and Small Breath is produced；Filter produce unload dirt waste water, separated produce vinasse it is equal
It is admitted to waste gas, waste liquid to remove the evil workshop section.
3. a kind of preparation method of antiglossing pigment aerosil as claimed in claim 2, it is characterised in that step 2)
Aerosil synthetic method is：
By step 1) SiCl after separated4、SiHCl3Or the CH for separately adding3SiCl3With steam heating gasified, with plus
The hydrogen that enters, excess air are fully reacted, and form aerosil and byproduct HCl；
Wherein, in course of reaction hydrogen portion derive from step 1) byproduct hydrogen gas；After reaction terminates, gas phase titanium dioxide will be contained
The gas of silicon is condensed by knockouts, then by the isolated aerosil of solid and gas；Then aerosil is steamed
Vapour carries out depickling process, carries out electrothermal drying, cooling after depickling again；Finally bulk density adjustment is carried out using volume machine；Step
2) solid and gas separation, depickling, the dry mix waste gas for producing are admitted to HCl recovery workshop section in.
4. a kind of preparation method of antiglossing pigment aerosil as claimed in claim 3, it is characterised in that in step
2) in the HCl recovery workshop section described in, step 2) in solid and gas separate, depickling and be dried the mix waste gas for producing and first pass through filter water
Remove a small amount of SiO of deentrainment2, after dedusting in gas HCl Jing concentration 21wt% hydrochloric acid solution three-level water absorption, formed it is dense
Spend the hydrochloric acid solution for 31wt%；The hydrochloric acid solution of the 31wt% of partially recycled gained loads storage tank export trade, remaining hydrochloric acid solution
Carry out de- analysis, the HCl for obtaining is used for step 1 Jing after the dehydration of the 98wt% concentrated sulfuric acids) silane synthesis；The hydrochloric acid of 31wt% after de- analysis
Solution concentration is dropped back to 21wt%, and fully recovering absorbs in HCl；
After the mix waste gas that filter is washed after dedusting, three-level water system absorb sequentially pass through again washing, two grades of alkali cleaning purifications,
The high aiutage high altitude discharges of Jing 25m, it is ensured that HCl concentration of emissions are not higher than 5ppm Jing after absorption cleaning；Hydrochloric acid tank Big and Small Breath
Storage tank breathing the washing with water of waste gas of generation, is re-fed into being discharged after caustic wash tower alkali cleaning purification；
Waste water after wherein above-mentioned washing is used as the water source of above-mentioned filter washing.
5. a kind of preparation method of antiglossing pigment aerosil as claimed in claim 4, it is characterised in that described
After the 98wt% concentrated sulfuric acids are dried to the HCl that de- analysis is obtained, the sulfuric acid of 90wt% is obtained, be deployed into dilute sulphur of 20wt%
After acid, use as the raw material of inorganic flocculating agent：After the sulfuric acid hybrid reaction of sodium metasilicate and 20wt%, aluminum sulfate, system are added
Into aluminium salt inorganic flocculating agent.
6. a kind of preparation method of antiglossing pigment aerosil as claimed in claim 1, it is characterised in that step 3)
Obtained delustring aerosil is also through modification：
A) weigh delustring aerosil and be configured to the suspension that concentration is 8-12wt%, separately compound concentration respectively
For the silver nitrate solution of 8-12wt%, magnesium nitrate solution and copper nitrate solution；Successively by silver nitrate solution, magnesium nitrate solution and nitre
Sour copper solution is added drop-wise in suspension and is uniformly dispersed, and obtains mixed liquor A；Wherein silver nitrate solution, magnesium nitrate solution and nitric acid
The consumption of copper solution is respectively 8-12%, 5-7%, 3-5% of suspension vol；
B) by tetraethyl orthosilicate, absolute ethyl alcohol and water by volume 1:4-6:2-3 mixes, and after stirring, is with concentration
It is 4-6 that the salpeter solution of 0.1mol/L adjusts pH, obtains mixed liquid B；Mixed liquor A is transferred in 50-55 DEG C of water-bath, in stirring
Under the conditions of mixed liquid B is added drop-wise in mixed liquor A, wherein the quality of mixed liquid B for mixed liquor A 4-8%；
C after) mixed liquid B is dripped, by product at 60-65 DEG C still aging 1-3h；Obtain modified silicon dioxide sol；
Modified silicon dioxide sol is dried at 100-110 DEG C, powder is then ground to, roasting 1-2h takes out at 400-600 DEG C, then
Modified delustring aerosil is obtained after secondary grinding.
7. a kind of preparation method of antiglossing pigment aerosil as claimed in claim 6, it is characterised in that step B)
In, the drop rate of mixed liquid B is 2-4mL/min.
8. a kind of preparation method of antiglossing pigment aerosil as claimed in claim 1, it is characterised in that step 3)
In, the specific surface area of the delustring aerosil for finally obtaining is 150 ± 20m2/g。
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| CN1817138A (en) * | 2006-03-16 | 2006-08-16 | 上海师范大学 | Silver-carried antibacterial agent with nanometer porous and making method thereof |
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Inventor after: Yang Xiaoyi Inventor after: Liu Guojing Inventor after: Tan Jun Inventor after: Zhao Yanyan Inventor after: Xu Huifen Inventor after: Fan Jianping Inventor before: Fang Weimin Inventor before: Tan Jun Inventor before: Liu Guojing Inventor before: Yang Xiaoyi Inventor before: Zhao Yanyan Inventor before: Liu Xiaolei Inventor before: Wang Jumei Inventor before: Xu Huifen Inventor before: Fan Jianping |
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