CN107445584A - A kind of preparation method of high intensity, porous water imbibition geo-polymer - Google Patents
A kind of preparation method of high intensity, porous water imbibition geo-polymer Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of high intensity, porous water imbibition geo-polymer, belong to geo-polymer preparing technical field.The present invention to material powder first by carrying out hydrophilic modifying, improve the water imbibition of oligomer, foamed again with self-control foaming agent, improve ground polymers internal bond strength, crystallization will be sintered again, and produce nano-silica film layer, further improve the mechanical strength of geo-polymer, and the present invention improves alkaline environment using caused alkali in foaming process, without another exogenously added alkali, it is cost-effective, the mechanical performance of geo-polymer is improved while porosity is kept, is had broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of high intensity, porous water imbibition geo-polymer, belongs to geo-polymer preparation
Technical field.
Background technology
Geo-polymer referred to as polymers, be that engineering material industry develops one of more active material recent years, also by
It is considered a kind of 21 century green gel material.Geo-polymer is a kind of to be generated in the basic conditions by aluminum silicate raw material
Inorganic polymer material, the country are also known as soil polyalcohol, mineral polymer, mineral polymeric material etc..Geology polymer material
With following feature：（1）Intensity is high, and its mechanical performance index is better than cement and concrete；（2）With stronger corrosion-resistant
Property, hydrothermal, high high-temp stability and preferable durability；（3）Wide material sources, cost are cheap；（4）Preparation technology is simple,
Molding mode is various, and plasticity is good.Research shows that the ground polymers porous material prepared by foaming has preferably water suction
Rate, in certain space, bubble caused by foaming agent causes to form perforate in sample and hole-closing structure, foaming agents content are got over
More, bubble is more, can form substantial amounts of pore structure, but a large amount of pore structures can seriously reduce the machinery of ground polymers based porous materials
Intensity.
Therefore, a kind of porous water-absorbing geo-polymer with high mechanical properties is invented to oligomeric materials technology of preparing
Field has positive meaning.
The content of the invention
Present invention mainly solves technical problem, although have for water imbibition geo-polymer made from current foaming
Preferable water imbibition, but increasing for pore structure causes the mechanical strength of geo-polymer to reduce, therefore invented a kind of high-strength
Spend the preparation method of porous water-absorbing geo-polymer.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of high intensity, porous water imbibition geo-polymer, it is characterised in that specifically preparation process is：
（1）Ground 200 mesh sieve after granite and kaolin are mixed, obtains mixed-powder, is soaked after soybean and water are mixed,
Soybean after immersion is put into soy bean milk making machine and is beaten, is filtrated to get soya-bean milk；
（2）Fermentation substrate is obtained after above-mentioned mixed-powder and soya-bean milk are mixed, then Grape Skin surface is rinsed with water, collects and rinses
Liquid, fermentation substrate is fitted into fermentation tank, then flushing liquor is added into fermentation tank, be sealed by fermentation, filtered after fermentation ends, separated
Filter residue is obtained, it is standby；
（3）Gum arabic heat temperature raising is made into its fusing, then the gum arabic after sodium peroxide powder and fusing is mixed
Stirring, stirring terminates rear natural cooling solidification, and is put into pulverizer and crushes, and obtains making foaming agent by oneself；
（4）Standby filter residue, sodium silicate solution and above-mentioned self-control foaming agent and ammonium chloride are mixed, obtain ground polymers slurry,
Ground polymers slurry and biogas slurry are mixed again, the iron mould that size is 20mm × 20mm × 20mm is injected after being stirred with agitator
In tool；
（5）After the completion for the treatment of above-mentioned injection, irony mould is put into greenhouse, maintenance is stood, the demoulding, it is thick to obtain foaming ground polymers
Product；
（6）By above-mentioned foaming polymers crude product is immersed in hydrochloric acid solution and taken out after 10~15min, and Muffle furnace is transferred to after naturally dry
In, after heat preservation sintering, discharging, produce high intensity, porous water imbibition geo-polymer.
Step（1）Described in granite and kaolinic mass ratio be 1:3, the mass ratio of soybean and water is 1：5, immersion
Time is 10~12h.
Step（2）Described in mixed-powder and soya-bean milk mass ratio be 1:3, addition and the fermentation substrate matter of flushing liquor
Measure it is equal, be sealed by fermentation temperature be 35~45 DEG C, be sealed by fermentation the time be 15~20 days.
Step（3）Described in sodium peroxide powder and the gum arabic after fusing mass ratio be 1:5.
Step（4）Described in filter residue, sodium silicate solution and self-control foaming agent and ammonium chloride mass ratio be 50:20:
1:1, the mass fraction of sodium silicate solution is 10%, and the quality of ground polymers slurry and biogas slurry is equal.
Step（5）Described in greenhouse temperature be 40~50 DEG C, relative air humidity be 70~80%, stand maintenance when
Between be 5~7 days.
Step（6）Described in the mass fraction of hydrochloric acid solution be 5%, the method for heat preservation sintering is：With 10 DEG C/min speed
Rate temperature programming is to 900~1000 DEG C, 2~4h of heat preservation sintering.
The beneficial effects of the invention are as follows：
（1）The present invention is using salic minerals mixed-powder as raw material, by itself and soya-bean milk mixed fermentation, using microorganism by soya-bean milk
For protein degradation into amino acid, amino acid produces carboxyl and amino after decomposing, and is grafted under the self-crosslinking of microorganism mixed
Powder surface is closed, so as to add mixed-powder surface hydrophilicity amino and carboxyl quantity, improves the hydrophily of mixed-powder,
The water absorbing properties that can cause final obtained geo-polymer in this, as raw material are greatly improved；
（2）The present invention is coated sodium peroxide with natural resin gum arabic, avoids it from directly being contacted with moisture, then by parent
The mixed-powder and cladded type sodium peroxide and sodium metasilicate, ammonium chloride that water is modified are mixed to prepare slurry, on the one hand utilize chlorination
Unstable sodium ion and potassium ion are combined in ammonium ion substitution mixed powder in ammonium so that interior during final oligomer shaping
Portion's firm binding force, the mechanical strength of oligomer is improved, in addition as the addition of waterglass, system pH rises, mixed-powder are molten
Solution amount increases, and calcium, magnesium ion and the silica Interaction of substituents discharged increases intergranular bridge joint effect degree, improved
The mechanical strength of oligomer；
（3）The present invention coats sodium peroxide as foaming agent by the use of gum arabic, recycles the biogas slurry rich in microorganism as dilute
Liquid is released, causes the sodium peroxide of cladding is exposed to be reacted with water contact with microorganism feeding natural resin gum arabic
Gas is produced, plays foaming effect, sodium hydroxide can be generated when sodium peroxide and water react in addition, alkalescence is provided for whole system
Environment, without addition alkali in addition, acid soak base substrate is used after shaping, precipitated using hydrochloric acid and sodium metasilicate reaction generation orthosilicic acid, most
After carry out ablation, the partially-crystallized anorthite high for mechanical strength of the geo-polymer after high-temperature process, and orthosilicic acid is heated
Be decomposed into it is nano-silica filled in the polymer, further increase the mechanical performance of geo-polymer.
Embodiment
It is 1 in mass ratio:3 will be fitted into ball mill after granite and kaolin mixing, and 200 mesh sieves are crossed after grinding 1~2h,
Mixed-powder is obtained, is 1 in mass ratio by soybean and water：10~12h is soaked after 5 mixing, the soybean after immersion is put into soya-bean milk
It is beaten in machine, is filtrated to get soya-bean milk；It is 1 in mass ratio by mixed-powder and soya-bean milk:Fermentation substrate is obtained after 3 mixing, then uses water
Grape Skin surface is rinsed, flushing liquor is collected, fermentation substrate is fitted into fermentation tank, then the matter such as fermentation substrate are added into fermentation tank
The flushing liquor of amount, tank mouth is sealed, is sealed by fermentation 15~20 days, is filtered after fermentation ends, isolated filter residue at 35~45 DEG C；
Gum arabic is heated into 80~90 DEG C makes its fusing, then is 1 in mass ratio:5 by after sodium peroxide powder and fusing
Gum arabic mix 20~30min, stirring terminates the solidification of rear natural cooling, and be put into pulverizer and crush 20~
30min, obtain making foaming agent by oneself；It is 50 in mass ratio:20:1:Filter residue, mass fraction are 10% sodium silicate solution and self-control by 1
Foaming agent and ammonium chloride mixing, stir 30~40min, obtain ground polymers slurry, then by ground polymers slurry and biogas slurry by etc. matter
Amount than mixing, after being stirred 15~20min using 300~400r/min rotating speeds with agitator inject size as 20mm × 20mm ×
In 20mm iron mould；After the completion of to be implanted, irony mould is put into temperature as 40~50 DEG C, relative air humidity is 70~
In 80% greenhouse, maintenance 5~7 days are stood, the demoulding, obtain foaming ground polymers crude product；Foaming ground polymers crude product is immersed into quality point
Number is to be taken out in 5% hydrochloric acid solution after 10~15min, is transferred to after naturally dry in Muffle furnace, with 10 DEG C/min rate program liter
Temperature is to 900~1000 DEG C, after 2~4h of heat preservation sintering, discharging, produces high intensity, porous water imbibition geo-polymer.
Example 1
It is 1 in mass ratio:3 will be fitted into ball mill after granite and kaolin mixing, cross 200 mesh sieves after grinding 1h, are mixed
Powder is closed, is 1 in mass ratio by soybean and water：10h is soaked after 5 mixing, the soybean after immersion is put into soy bean milk making machine and is beaten, mistake
Filter obtains soya-bean milk；It is 1 in mass ratio by mixed-powder and soya-bean milk:Fermentation substrate is obtained after 3 mixing, then grape epidermis is rinsed with water
Face, flushing liquor is collected, fermentation substrate is fitted into fermentation tank, then the flushing liquor of the quality such as fermentation substrate is added into fermentation tank,
Tank mouth is sealed, is sealed by fermentation 15 days, is filtered after fermentation ends, isolated filter residue at 35 DEG C；Gum arabic is heated and risen
Warm to 80 DEG C make its fusing, then are 1 in mass ratio:5 mix the gum arabic after sodium peroxide powder and fusing
20min, stirring terminates rear natural cooling solidification, and is put into pulverizer and crushes 20min, obtains making foaming agent by oneself；In mass ratio
For 50:20:1:Filter residue, mass fraction are 10% sodium silicate solution and make foaming agent and ammonium chloride mixing, stirring by oneself by 1
30min, ground polymers slurry is obtained, then by ground polymers slurry and biogas slurry by waiting mass ratio to mix, with agitator with 300r/min turns
Speed is injected in the iron mould that size is 20mm × 20mm × 20mm after being stirred 15min；After the completion of to be implanted, by irony mould
Tool is put into temperature as 40 DEG C, and relative air humidity is in 70% greenhouse, stands maintenance 5 days, the demoulding, it is thick to obtain foaming ground polymers
Product；It is to be taken out in 5% hydrochloric acid solution after 10min that foaming ground polymers crude product is immersed into mass fraction, and Muffle furnace is transferred to after naturally dry
In, it is warming up to 900 DEG C with 10 DEG C/min rate program, after heat preservation sintering 2h, discharging, produces high intensity, porous water imbibition geology
Polymer.
Example 2
It is 1 in mass ratio:3 will be fitted into ball mill after granite and kaolin mixing, cross 200 mesh sieves after grinding 2h, are mixed
Powder is closed, is 1 in mass ratio by soybean and water：11h is soaked after 5 mixing, the soybean after immersion is put into soy bean milk making machine and is beaten, mistake
Filter obtains soya-bean milk；It is 1 in mass ratio by mixed-powder and soya-bean milk:Fermentation substrate is obtained after 3 mixing, then grape epidermis is rinsed with water
Face, flushing liquor is collected, fermentation substrate is fitted into fermentation tank, then the flushing liquor of the quality such as fermentation substrate is added into fermentation tank,
Tank mouth is sealed, is sealed by fermentation 18 days, is filtered after fermentation ends, isolated filter residue at 40 DEG C；Gum arabic is heated and risen
Warm to 85 DEG C make its fusing, then are 1 in mass ratio:5 mix the gum arabic after sodium peroxide powder and fusing
25min, stirring terminates rear natural cooling solidification, and is put into pulverizer and crushes 25min, obtains making foaming agent by oneself；In mass ratio
For 50:20:1:Filter residue, mass fraction are 10% sodium silicate solution and make foaming agent and ammonium chloride mixing, stirring by oneself by 1
35min, ground polymers slurry is obtained, then by ground polymers slurry and biogas slurry by waiting mass ratio to mix, with agitator with 350r/min turns
Speed is injected in the iron mould that size is 20mm × 20mm × 20mm after being stirred 18min；After the completion of to be implanted, by irony mould
Tool is put into temperature as 45 DEG C, and relative air humidity is in 75% greenhouse, stands maintenance 6 days, the demoulding, it is thick to obtain foaming ground polymers
Product；It is to be taken out in 5% hydrochloric acid solution after 13min that foaming ground polymers crude product is immersed into mass fraction, and Muffle furnace is transferred to after naturally dry
In, it is warming up to 950 DEG C with 10 DEG C/min rate program, after heat preservation sintering 3h, discharging, produces high intensity, porous water imbibition geology
Polymer.
Example 3
It is 1 in mass ratio:3 will be fitted into ball mill after granite and kaolin mixing, cross 200 mesh sieves after grinding 2h, are mixed
Powder is closed, is 1 in mass ratio by soybean and water：12h is soaked after 5 mixing, the soybean after immersion is put into soy bean milk making machine and is beaten, mistake
Filter obtains soya-bean milk；It is 1 in mass ratio by mixed-powder and soya-bean milk:Fermentation substrate is obtained after 3 mixing, then grape epidermis is rinsed with water
Face, flushing liquor is collected, fermentation substrate is fitted into fermentation tank, then the flushing liquor of the quality such as fermentation substrate is added into fermentation tank,
Tank mouth is sealed, is sealed by fermentation 20 days, is filtered after fermentation ends, isolated filter residue at 45 DEG C；Gum arabic is heated and risen
Warm to 90 DEG C make its fusing, then are 1 in mass ratio:5 mix the gum arabic after sodium peroxide powder and fusing
30min, stirring terminates rear natural cooling solidification, and is put into pulverizer and crushes 30min, obtains making foaming agent by oneself；In mass ratio
For 50:20:1:Filter residue, mass fraction are 10% sodium silicate solution and make foaming agent and ammonium chloride mixing, stirring by oneself by 1
40min, ground polymers slurry is obtained, then by ground polymers slurry and biogas slurry by waiting mass ratio to mix, with agitator with 400r/min turns
Speed is injected in the iron mould that size is 20mm × 20mm × 20mm after being stirred 20min；After the completion of to be implanted, by irony mould
Tool is put into temperature as 50 DEG C, and relative air humidity is in 80% greenhouse, stands maintenance 7 days, the demoulding, it is thick to obtain foaming ground polymers
Product；It is to be taken out in 5% hydrochloric acid solution after 15min that foaming ground polymers crude product is immersed into mass fraction, and Muffle furnace is transferred to after naturally dry
In, it is warming up to 1000 DEG C with 10 DEG C/min rate program, after heat preservation sintering 4h, discharging, with producing high intensity, porous water imbibition
Matter polymer.
Reference examples
Reference examples are used as using the geo-polymer of Shanghai City company production
The geo-polymer of example and reference examples is detected, specific detection is as follows：
1. water absorption rate determines：The water absorption rate of geo-polymer is tested according to standard GB/T 3810.3-2006；
2. rupture strength determines：Rupture strength after geo-polymer conserves 7 days is tested according to standard GB/T 3810.4-2006；
3. compressive strength determination：Compression strength after being conserved 7 days according to GB/T50107 standard testings geo-polymer.
Test result is as shown in table 1：
Table 1
Geo-polymer produced by the present invention has a splendid mechanical performance it can be seen from data in upper table, and application prospect is wide
It is wealthy.
Claims (7)
1. a kind of preparation method of high intensity, porous water imbibition geo-polymer, it is characterised in that specifically preparation process is：
（1）Ground 200 mesh sieve after granite and kaolin are mixed, obtains mixed-powder, is soaked after soybean and water are mixed,
Soybean after immersion is put into soy bean milk making machine and is beaten, is filtrated to get soya-bean milk；
（2）Fermentation substrate is obtained after above-mentioned mixed-powder and soya-bean milk are mixed, then Grape Skin surface is rinsed with water, collects and rinses
Liquid, fermentation substrate is fitted into fermentation tank, then flushing liquor is added into fermentation tank, be sealed by fermentation, filtered after fermentation ends, separated
Filter residue is obtained, it is standby；
（3）Gum arabic heat temperature raising is made into its fusing, then the gum arabic after sodium peroxide powder and fusing is mixed
Stirring, stirring terminates rear natural cooling solidification, and is put into pulverizer and crushes, and obtains making foaming agent by oneself；
（4）Standby filter residue, sodium silicate solution and above-mentioned self-control foaming agent and ammonium chloride are mixed, obtain ground polymers slurry,
Ground polymers slurry and biogas slurry are mixed again, the iron mould that size is 20mm × 20mm × 20mm is injected after being stirred with agitator
In tool；
（5）After the completion for the treatment of above-mentioned injection, irony mould is put into greenhouse, maintenance is stood, the demoulding, it is thick to obtain foaming ground polymers
Product；
（6）By above-mentioned foaming polymers crude product is immersed in hydrochloric acid solution and taken out after 10~15min, and Muffle furnace is transferred to after naturally dry
In, after heat preservation sintering, discharging, produce high intensity, porous water imbibition geo-polymer.
A kind of 2. preparation method of high intensity, porous water imbibition geo-polymer according to claim 1, it is characterised in that
Step（1）Described in granite and kaolinic mass ratio be 1:3, the mass ratio of soybean and water is 1：5, soak time 10
~12h.
A kind of 3. preparation method of high intensity, porous water imbibition geo-polymer according to claim 1, it is characterised in that
Step（2）Described in mixed-powder and soya-bean milk mass ratio be 1:3, the addition of flushing liquor is equal with fermentation substrate quality,
It is 35~45 DEG C to be sealed by fermentation temperature, and it is 15~20 days to be sealed by fermentation the time.
A kind of 4. preparation method of high intensity, porous water imbibition geo-polymer according to claim 1, it is characterised in that
Step（3）Described in sodium peroxide powder and the gum arabic after fusing mass ratio be 1:5.
A kind of 5. preparation method of high intensity, porous water imbibition geo-polymer according to claim 1, it is characterised in that
Step（4）Described in filter residue, sodium silicate solution and self-control foaming agent and ammonium chloride mass ratio be 50:20:1:1, silicic acid
The mass fraction of sodium solution is 10%, and the quality of ground polymers slurry and biogas slurry is equal.
A kind of 6. preparation method of high intensity, porous water imbibition geo-polymer according to claim 1, it is characterised in that
Step（5）Described in greenhouse temperature be 40~50 DEG C, relative air humidity be 70~80%, stand curing time be 5~7
My god.
A kind of 7. preparation method of high intensity, porous water imbibition geo-polymer according to claim 1, it is characterised in that
Step（6）Described in the mass fraction of hydrochloric acid solution be 5%, the method for heat preservation sintering is：With 10 DEG C/min rate program liter
Warm to 900~1000 DEG C, 2~4h of heat preservation sintering.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218314A (en) * | 2017-12-30 | 2018-06-29 | 姜向军 | A kind of preparation method of high plasticity bone porcelain pug |
| CN108499372A (en) * | 2018-03-28 | 2018-09-07 | 何治伟 | A method of preparing high tenacity porous ceramic film support using microorganism |
| CN110372326A (en) * | 2019-06-12 | 2019-10-25 | 魏炎梅 | A kind of preparation method of heatproof and shockproof ceramic filtering material |
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| CN110372326A (en) * | 2019-06-12 | 2019-10-25 | 魏炎梅 | A kind of preparation method of heatproof and shockproof ceramic filtering material |
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