CN105800623A - Method for preparing silicon dioxide aerogel heat insulation material at low cost with industrial waste residues of pipeline residues in phosphate fertilizer plants as raw materials - Google Patents
Method for preparing silicon dioxide aerogel heat insulation material at low cost with industrial waste residues of pipeline residues in phosphate fertilizer plants as raw materials Download PDFInfo
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- CN105800623A CN105800623A CN201610180000.3A CN201610180000A CN105800623A CN 105800623 A CN105800623 A CN 105800623A CN 201610180000 A CN201610180000 A CN 201610180000A CN 105800623 A CN105800623 A CN 105800623A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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Abstract
The invention relates to a method for preparing a silicon dioxide aerogel heat insulation material at low cost with industrial waste residues of pipeline residues in phosphate fertilizer plants as raw materials and belongs to the technical field of aerogel materials.The method comprises the steps that firstly, silicon oxide in the pipeline residues is extracted with an alkali dissolution method, a sodium silicate solution is obtained and subjected to ion exchange through 732 cation exchange resin, and sol is obtained; after the pH of the sol is titrated with an alkali solution, standing is carried out for obtaining gel; the gel is subjected to aging, solvent exchange with ethanol and n-hexan and hydrophobization treatment, finally drying is carried out at the normal pressure, and silicon dioxide aerogel is obtained.The material has good hydrophobicity, a good pore structure and good heat preservation performance.
Description
Technical field
The present invention designs the technology of preparing of a kind of low cost aerosil heat-barrier material.
Background technology
Aeroge is referred to as the lightest transparent solid, and it is one kind of low density solid-state material.By by gel
Liquid in space air substitutes, and network structure during gel state is maintained simultaneously, is so obtained
Material become aeroge.Owing to aerosil has high-specific surface area, high porosity, loud
The features such as impedance, low-density, low thermal conductivity, it is increasingly widely used in high-velocity particles and is caught
Device, catalyst, soundproof wall, nuclear fusion target and building heat preservation field.Due to aerosil
Hole dimension is less than air molecule mean free path under normal pressure, and therefore in aeroge, air molecule is close to static,
Thus the heat transfer that the cross-ventilation avoided produces.On the other hand, aerosil has extremely low
The crooked route of bulk density and Specific surface area also prevents the heat transfer of gaseous state and solid-state, furthermore,
Tending to infinite many hole walls, that heat radiation can be made to be down to is minimum.The common effect of above three aspects, almost hinders
All paths of heat transfer of having broken, make aeroge reach the insulation effect that other materials is incomparable.But want
Realize the aerosil application in building energy saving field, except requiring the performance such as heat insulation of aeroge
Outside up to standard, in addition it is also necessary to realize the low cost manufacture of aerogel material, this following aerosil just
The important development trend of research.
The manufacturing cost of aerosil is concentrated mainly on presoma, chemical levels and is dried
In technique, the mistake that during especially the usage amount of silane coupler is aeroge preparation process, cost is the highest
Journey.Prepare aerosil raw material at present using most is methyl silicate, tetraethyl orthosilicate etc.
The presoma of silanol salt, but these presomas are expensive, and some also has toxicity.For rice husk
The presoma of the silicic acid sodium form such as ash, flyash, although the cost of raw material can significantly decline, but for
Raw-material process work is again tediously long and loaded down with trivial details.The method of supercritical drying is prepared during aeroge requires
The highest temperature and pressure, though more gentle CO2The supercritical drying flowing water to modernization
Line remains a bottleneck for producing.Consider from equipment cost of installation and maintenance, the method for constant pressure and dry
Prepare aeroge, be the development trend of following aeroge.But constant pressure and dry needs the solvent carrying out multistep to hand over
Change, need the processing stage of hydrophobization to use substantial amounts of silane coupler to modify wet gel, the preparation saved
The production cost that cost brings not as good as silane coupler luxus consumption far away improves.Therefore in constant pressure and dry mistake
How Cheng Zhong, reduce organic solvent and silane coupler in the case of ensureing aeroge properties
Consumption is one of the direction that should deeply probe into of researcher.
Summary of the invention
It is an object of the invention to provide a kind of trade waste phosphate fertilizer plant pipeline slag is cheap silicon source, system
The method of the silica aerogel material of standby excellent performance.Using a kind of new presoma as silicon source, no
But reduce the preparation cost of material, more solve the harm that environment is caused by the bulk deposition of pipeline slag.
Additionally being kept to twice by the exchange times of ethanol during solvent exchange, the exchange times of normal hexane subtracts
Few for once；Hydrophobization processing procedure reduces the consumption of silane coupler, the most enough ensures aeroge material
The heat conductivity of material.From constant pressure and dry, garbage as silicon source and the usage amount of reduction silane coupler
Three aspects reduce the preparation cost of material.The present invention solves high the asking of cost in aeroge preparation process
Topic, the performance of aeroge does not reduce simultaneously.
For solving above-mentioned technical problem, the present invention is carried out as steps described below:
(1) the pipeline slag after washing and strong base solution are mixed, after mix homogeneously, at normal pressure
Under heat, finally filter；
(2) filtrate after filtering carries out ion exchange through 732 cation exchange resiies, obtains
PH value Ludox between 2-3, adds base catalyst, the pH to 5-6 of regulation Ludox；
(3) the colloidal sol heating in water bath gelation obtaining step (2), the bath temperature of gel is 30 DEG C
-50 DEG C, the gel of formation is aging at 30-50 DEG C, respectively with dehydrated alcohol, the exchange of normal hexane reagent
Remove the water in gel, ethanol, obtain wet gel X；
(4) silane coupler is used with the mixed solution of dehydrated alcohol, normal hexane, step (3) to be obtained
To wet gel X carry out hydrophobization process, obtain wet gel Y；
(5) the wet gel Y normal hexane that step (4) obtains is embathed, obtain wet gel Z；
(6) the wet gel Z that step (5) obtains is dried at ambient pressure obtains silicon dioxide airsetting
Glue.
Step 1) in, described pipeline slag removes oxide impurity through washing, and washing times is 4 times,
The industrial residue being finally dried to obtain, baking temperature is 110 DEG C, drying time 3h-5h.
Step 1) in, described strong base solution is at least one in sodium hydroxide, potassium hydroxide, and highly basic is dense
Degree is 2mol/L-4mol/L, and strong base solution is 4-8:1L/kg with the ratio of pipeline slag；Described temperature controls
80 DEG C-100 DEG C, the described heated and stirred time is 2h-4h.
Step 2) in, described base catalyst is NH3·H2O solution, described NH3·H2O solution
Concentration be 1mol/L～3mol/L.
Step 3) in, the described aging time is 12h-24h；The time of described ethanol exchange is 12h,
Every 4h-6h changes once；The time of described normal hexane exchange is 12h, and every 4h-12h changes once；；(institute
The swap time stated is that solvent continues swap time, and every 4h-6h changes and once refers to what every 4h-6h more renewed
Solvent, the following stated swap time and number of times are this implication) ethanol with the volume ratio of wet gel is
1:1-3:1, normal hexane is 1:1-3:1 with the volume ratio of wet gel.
Step 4) in, silane coupler is trim,ethylchlorosilane, trimethylmethoxysilane, hexamethyl two
In silazane at least one, silane coupler is 1:1-3:1 with the ratio of the amount of the material of dehydrated alcohol, silane
Coupling agent is 0.25:1-1:1 with the ratio of the amount of the material of silicon dioxide in wet gel, and silane coupler is with just own
The volume ratio of alkane is 1:25-3:25, and the time that hydrophobization processes is 6h-24h, and temperature controls at 30 DEG C
-50℃。
Step 5) in, described normal hexane embathe remove by-product time be 12h, embathe temperature control
At 30-50 DEG C.
Step 6) in, described constant pressure and dry, dry temperature and time is to be dried 1h at 50 DEG C respectively,
200 DEG C of dry 1h.
Beneficial effect:
The inventive method is carried out at normal temperatures and pressures, and constant pressure and dry makes the cost of equipment greatly be dropped
Low, there is safety；Using pipeline slag is silicon source so that cost of material is reduced, and solves
The environmental problem that pipeline slag muck manufactures；Reducing the exchange times of solvent exchange procedure solvent, reduction shows
In modifying process, the usage amount of silane coupler, reduces preparation cost.And use said method to prepare
The aeroge obtained has good heat-proof quality.
Detailed description of the invention
In order to introduce technical scheme in more detail, below carry out specific embodiment, but
Present disclosure is not limited to following example.
Embodiment 1
(1) by pipeline slag distilled water wash 4 times, and under the conditions of 110 DEG C, 4h it is dried.Take 10g water
After pipeline slag after washing and 160ml 2mol/L NaOH solution mix homogeneously, heat at ambient pressure,
Temperature controls at 100 DEG C, and heat time heating time, 2h, finally filtered；(2) filtrate after filtering is passed through
732 cation exchange resiies carry out ion exchange, obtain the Ludox that pH value is 2.49, add 1mol/L
NH3·H2O solution is as base catalyst, the pH to 5.52 of regulation Ludox；(3) to step (2)
The colloidal sol heating in water bath gelation obtained, the bath temperature of gel is 50 DEG C, and the gel of formation is at 50 DEG C
Aging 12h, removes the water in gel, ethanol with dehydrated alcohol, the exchange of normal hexane reagent respectively；Ethanol is handed over
The time changed is 12h, and every 4h changes once；The time of normal hexane exchange is 12h, and every 4h changes once；Second
Alcohol is 1:1 with the volume ratio of wet gel, and normal hexane is 1:1 with the volume ratio of wet gel, and temperature controls
50 DEG C, obtain wet gel X；(4) use trim,ethylchlorosilane molten with the mixing of dehydrated alcohol, normal hexane
Liquid carries out hydrophobization process, trim,ethylchlorosilane and dehydrated alcohol to the wet gel X that step (3) obtains
The ratio of the amount of material is 1:1, and trim,ethylchlorosilane with the ratio of the amount of the material of silicon dioxide in wet gel X is
1:1, trim,ethylchlorosilane is 1:25 with the volume ratio of normal hexane, and the time that hydrophobization processes is 24h, temperature
Degree controls to obtain wet gel Y at 50 DEG C；(5) the wet gel Y normal hexane 50 DEG C that step (4) is obtained
Embathe 12h, obtain wet gel Z；(6) the wet gel Z that step (5) obtains is dried at ambient pressure
Obtain aerosil, baking temperature and time be respectively at 50 DEG C be dried 1h, 200 DEG C of dry 1h.
The aerosil pore structure prepared is good, and specific surface area is 432.39m2/ g, pore volume is
3.22cm3/ g, heat conductivity is 0.00801W/ (m K), and the contact angle to water is 164.3 °.
Embodiment 2
(1) by pipeline slag distilled water wash 4 times, and under the conditions of 110 DEG C, 4h it is dried.Take 10g water
After pipeline slag after washing and 160ml 2mol/L NaOH solution mix homogeneously, heat at ambient pressure,
Temperature controls at 100 DEG C, and heat time heating time, 2h, finally filtered；(2) filtrate after filtering is passed through
732 cation exchange resiies carry out ion exchange, obtain the Ludox that pH value is 2.56, add 1mol/L
NH3·H2O solution is as base catalyst, the pH to 5.46 of regulation Ludox；(3) to step (2)
The colloidal sol heating in water bath gelation obtained, the bath temperature of gel is 50 DEG C, and the gel of formation is at 50 DEG C
Aging 12h, removes the water in gel, ethanol with dehydrated alcohol, the exchange of normal hexane reagent respectively；Ethanol is handed over
The time changed is 12h, and every 6h changes once；The time of normal hexane exchange is 12h, and exchange is once altogether；Second
Alcohol is 1:1 with the volume ratio of wet gel, and normal hexane is 1:1 with the volume ratio of wet gel, and temperature controls
50 DEG C, obtain wet gel X；(4) use trim,ethylchlorosilane molten with the mixing of dehydrated alcohol, normal hexane
Liquid carries out hydrophobization process, trim,ethylchlorosilane and dehydrated alcohol to the wet gel X that step (3) obtains
The ratio of the amount of material is 1:1, and trim,ethylchlorosilane with the ratio of the amount of the material of silicon dioxide in wet gel X is
1:1, trim,ethylchlorosilane is 1:25 with the volume ratio of normal hexane, and the time that hydrophobization processes is 24h, temperature
Degree controls to obtain wet gel Y at 50 DEG C；(5) the wet gel Y normal hexane 30 DEG C that step (4) is obtained
Embathe 12h, obtain wet gel Z；(6) the wet gel Z that step (5) obtains is dried at ambient pressure
Obtain aerosil, baking temperature and time be respectively at 50 DEG C be dried 1h, 200 DEG C of dry 1h.
The exchange times of ethanol in step (3) is reduced to twice by this example, and the exchange times of normal hexane subtracts
Being 1 time less, the aerosil pore structure prepared is good, and specific surface area is 381.51m2/ g,
Pore volume is 3.17cm3/ g, heat conductivity is 0.0087W/ (m K), and the contact angle to water is 153.6 °.When
Just can by substantial amounts of water coke slurry in wet gel X hole out when ethanol exchange times is twice so that in hole
Water will not in hydrophobization processing procedure with trim,ethylchlorosilane generation hydrolysis.The exchange of normal hexane time
Can by a part of ethanol replacement in wet gel X out, but remain in wet gel X hole when number is one time
Ethanol, in hydrophobization processing procedure will not on wet gel Y produce impact.In conjunction with above-mentioned analysis, will
In step (3), the exchange times of ethanol is reduced to twice, and the exchange times of normal hexane is reduced to 1 time, greatly
The consumption having saved greatly chemical reagent reduces cost.
Embodiment 3
(1) by acidity pipeline slag with distilled water wash 4 times to neutral, and under the conditions of 110 DEG C, be dried 4h.
After taking the pipeline slag after 10g washing and 160ml 2mol/L NaOH solution mix homogeneously, enter at ambient pressure
Row heating, temperature controls at 100 DEG C, and heat time heating time, 2h, finally filtered；(2) after filtering
Filtrate carries out ion exchange through 732 cation exchange resiies, obtains the Ludox that pH value is 2.78,
Add 1mol/L NH3·H2O solution is as base catalyst, the pH to 5.42 of regulation Ludox；(3)
The colloidal sol heating in water bath gelation obtaining step (2), the bath temperature of gel is 50 DEG C, coagulating of formation
Glue is aging 12h at 50 DEG C, respectively with dehydrated alcohol, the exchange of normal hexane reagent remove the water in gel,
Ethanol；The time of ethanol exchange is 12h, and every 6h changes once；The time of normal hexane exchange is 12h, altogether
Exchange is once；Ethanol is 1:1 with the volume ratio of wet gel, and normal hexane is 1:1 with the volume ratio of wet gel,
Temperature controls, at 50 DEG C, to obtain wet gel X；(4) use trim,ethylchlorosilane and dehydrated alcohol, just oneself
The mixed solution of alkane carries out hydrophobization process to the wet gel X that step (3) obtains, trim,ethylchlorosilane with
The ratio of the amount of the material of dehydrated alcohol is 1:1, trim,ethylchlorosilane and the material of silicon dioxide in wet gel X
The ratio of amount be 0.5:1, trim,ethylchlorosilane is 1:25 with the volume ratio of normal hexane, hydrophobization process time
Between be 6h, temperature controls to obtain wet gel Y at 50 DEG C；(5) wet gel Y step (4) obtained uses
Normal hexane 30 DEG C embathes 12h, obtains wet gel Z；(6) wet gel Z step (5) obtained is at normal pressure
Under be dried and obtain aerosil, baking temperature and time are to be dried 1h at 50 DEG C respectively,
200 DEG C of dry 1h.
This example is by trim,ethylchlorosilane in step (4) and the amount of the material of silicon dioxide in wet gel X
Than being reduced to 0.5:1, the hydrophobization process time is reduced to 6h, the aerosil hole knot prepared
Structure is good, and specific surface area is 419.62m2/ g, pore volume is 3.44cm3/ g, heat conductivity is 0.009W/
(m K), the contact angle to water is 148.5 °.Silane coupler and dioxy in wet gel X in step (4)
The ratio 0.5:1 of the amount of the material of SiClx is fully sufficient, and the time that hydrophobization processes is reduced to 6h, made
Standby aeroge either pore structure, heat conductivity and hydrophobic performance vary less.Will step in this example
Suddenly in (4), trim,ethylchlorosilane is reduced to 0.5:1 with the ratio of the amount of the material of silicon dioxide in wet gel X,
It is greatly saved the usage amount of silane coupler, reduces cost.
Claims (8)
1. one kind with industrial residue--and phosphate fertilizer plant's pipeline slag is that raw material low cost prepares silicon dioxide
The method of aerogel heat-insulating material, it is characterised in that carry out in the steps below:
(1) the pipeline slag after washing and strong base solution are mixed, after mix homogeneously, often
Pressure is heated, and finally filters；
(2) filtrate after filtering carries out ion exchange through 732 cation exchange resiies,
To pH value Ludox between 2-3, adding base catalyst, the pH of regulation Ludox is extremely
5-6；
(3) the colloidal sol heating in water bath gelation obtaining step (2), the bath temperature of gel is
30-50 DEG C, the gel of formation is aging at 30-50 DEG C, respectively with dehydrated alcohol, normal hexane reagent
The water in gel, ethanol are removed in exchange, obtain wet gel X；
(4) use silane coupler and dehydrated alcohol, normal hexane mixed solution to step (3)
The wet gel X obtained carries out hydrophobization process, obtains wet gel Y；
(5) the wet gel Y normal hexane that step (4) obtains is embathed, obtain wet gel Z；
(6) the wet gel Z that step (5) obtains is dried at ambient pressure obtains silicon dioxide gas
Gel.
2. a kind of with industrial residue--phosphate fertilizer plant's pipeline slag is raw material low cost
The method preparing aerosil heat-barrier material, it is characterised in that step 1) in, described
Pipeline slag removes oxide impurity through washing, and washing times is 4 times, the work being finally dried to obtain
Industry waste residue, baking temperature is 110 DEG C, drying time 3h-5h.
3. a kind of with industrial residue--phosphate fertilizer plant's pipeline slag is raw material low cost
The method preparing aerosil heat-barrier material, it is characterised in that step 1) in, described
Strong base solution is at least one in sodium hydroxide, potassium hydroxide, and strong base concentrations is 2mol/L-4mol/L,
Strong base solution is 4-8:1L/kg with the ratio of pipeline slag；Described temperature controls at 80 DEG C-100 DEG C, institute
Stating the heated and stirred time is 2h-4h.
4. a kind of with industrial residue--phosphate fertilizer plant's pipeline slag is raw material low cost
The method preparing aerosil heat-barrier material, it is characterised in that step 2) in, described
Base catalyst is NH3·H2O solution, described NH3·H2The concentration of O solution be 1mol/L～
3mol/L。
5. a kind of with industrial residue--phosphate fertilizer plant's pipeline slag is raw material low cost
The method preparing aerosil heat-barrier material, it is characterised in that step 3) in, described always
The time changed is 12h-24h；The time of described ethanol exchange is 12h, and every 4h-6h changes once；Institute
The time stating normal hexane exchange is 12h, and every 4h-12h changes once；Ethanol and the volume of wet gel X
Ratio is 1:1-3:1, and normal hexane is 1:1-3:1 with the volume ratio of wet gel Y.
6. a kind of with industrial residue--phosphate fertilizer plant's pipeline slag is raw material low cost
The method preparing aerosil heat-barrier material, it is characterised in that step 4) in, silane is even
Connection agent is at least one in trim,ethylchlorosilane, trimethylmethoxysilane, hexamethyldisiloxane,
Silane coupler is 1:1-3:1, silane coupler and wet gel with the ratio of the amount of the material of dehydrated alcohol
The ratio of the amount of the material of Z is 0.25:1-1:1, and silane coupler with the volume ratio of normal hexane is
1:25-3:25, the time that hydrophobization processes is 6h-24h, and temperature controls at 30 DEG C-50 DEG C.
7. a kind of with industrial residue--phosphate fertilizer plant's pipeline slag is raw material low cost
The method preparing aerosil heat-barrier material, it is characterised in that step 5) in, described
Normal hexane embathe remove by-product time be 12h, embathe temperature and control at 30 DEG C-50 DEG C.
8. a kind of with industrial residue--phosphate fertilizer plant's pipeline slag is raw material low cost
The method preparing aerosil heat-barrier material, it is characterised in that step 6) in, described
Constant pressure and dry, dry temperature and time is to be dried 1h, 200 DEG C of dry 1h at 50 DEG C respectively.
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| CN106745000A (en) * | 2016-12-23 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of preparation method of waterglass base aerosil |
| CN109911906A (en) * | 2019-03-28 | 2019-06-21 | 内蒙古工业大学 | A method of hydrophobic silica is prepared using zirconium metallurgical slag |
| CN110127707A (en) * | 2019-06-12 | 2019-08-16 | 云南凯威特新材料股份有限公司 | A method of high hydrophobicity aerosil is prepared with product silica gel in phosphate fertilizer industry |
| CN113336231A (en) * | 2021-06-30 | 2021-09-03 | 同济大学 | Method for preparing aerogel by taking municipal incineration waste ash as raw material through normal pressure drying |
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| CN106745000A (en) * | 2016-12-23 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of preparation method of waterglass base aerosil |
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