CN1031749C - Production process of silica gel and silica gel product thereof - Google Patents
Production process of silica gel and silica gel product thereof Download PDFInfo
- Publication number
- CN1031749C CN1031749C CN 93110232 CN93110232A CN1031749C CN 1031749 C CN1031749 C CN 1031749C CN 93110232 CN93110232 CN 93110232 CN 93110232 A CN93110232 A CN 93110232A CN 1031749 C CN1031749 C CN 1031749C
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- Prior art keywords
- silica gel
- former
- micelles
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000000741 silica gel Substances 0.000 title claims abstract description 43
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 8
- 230000020477 pH reduction Effects 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 3
- 229920001971 elastomer Polymers 0.000 claims description 16
- 239000005060 rubber Substances 0.000 claims description 16
- 239000000693 micelle Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 5
- 239000002585 base Substances 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000003929 acidic solution Substances 0.000 claims description 3
- 230000000274 adsorptive effect Effects 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- FGZJXVSDDHVZAH-UHFFFAOYSA-N ethoxyethane silane Chemical compound [SiH4].CCOCC FGZJXVSDDHVZAH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 235000011194 food seasoning agent Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 150000003568 thioethers Chemical class 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 4
- 230000004913 activation Effects 0.000 abstract description 2
- 238000001994 activation Methods 0.000 abstract description 2
- 239000000017 hydrogel Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000032683 aging Effects 0.000 abstract 1
- 238000005336 cracking Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000001879 gelation Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 206010016825 Flushing Diseases 0.000 description 1
- 208000033830 Hot Flashes Diseases 0.000 description 1
- 206010060800 Hot flush Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a production process of B-type silica gel and a product thereof. The process adopts a rotary mixed spherical silica gel granulating device to prepare spherical hydrogel silica gel, and then adopts a series of treatment processes of aging, acidification, water washing, activation, drying and the like to ensure that the average pore diameter of the silica gel is 0.004-0.007 mu and the specific surface area is 400-700 m2(ii)/g, the average particle size is 1-8 mm. The silica gel is more suitable for being used as a raw material of the fragrant silica gel and has the advantage of not cracking when meeting water.
Description
The invention discloses a kind of silica gel production technique, especially a kind of producing and manufacturing technique of Type B silica gel and silica gel product thereof, it belongs to technical field of inorganic chemical industry.
Commercially available silica gel by its hole classification, has silochrom and Kiselgel A.This two classes silica gel has can be used as siccative, moisture adsorbent, and sorbent material uses, and what have can be used as various reaction support of the catalyst, and what have can be used as the chromatographic column packing material.These silica gel are because the structure difference of its gel skeleton, the granularity difference, and hole geometry difference, and show difference on the bigger performance.Yet these silica gel all have a shortcoming that the common defective-chance water bursts.This is reason wherein, is exactly the inner skeleton insufficient strength of silica gel, and the aperture of internal void excessive (0.008～0.01 μ) or too small (0.001～0.004 μ) influence frame strength.The Kiselgel A of a kind of chromatographic column with weighting agent arranged, its manufacture method, 62-278113 is disclosed as day disclosure special permission communique: " generate in the silica gel process at silicon sol, its gelation reaction is to carry out in the dispersion agent of organic solvent and nonionogenic tenside formation ".The aftertreatment of its " gelation finish back " be " through filtration, clean, drying finally makes silica gel." in other words, the gelation in dispersant system of its silica gel, i.e. emulsification-gelation-molding, granulating.Wherein the organic solvent of dispersant system and tensio-active agent role are " raising mixing effect " " emulsification is gelation thereafter " this dynamichandling, be unfavorable for that the silica gel skeleton structure becomes to become strong admittedly, Gu the mean pore size of this its silica gel exists: 2～30A (0.0002～0.003 μ).
The Type B silica gel and the method for manufacturing technology thereof that will provide a kind of skeleton structure strong is provided.This processing method is made spherical water-setting silica gel by the air prilling device, carries out a series of aftertreatment technologys again, makes Type B silica gel.Its frame strength is improved, meet water and do not burst, control its aperture and exist: 0.004～0.007 μ, specific surface area is at 400～700m
2/ g, mean particle size is at 1～8mm, and adsorptive capacity is (60～80) % under relative humidity 90% situation.
Task of the present invention is that following scheme realizes: at first adopt traditional adhesive-preparing technology.Here it is by sodium silicate aqueous solution and dilution heat of sulfuric acid, and through the reaction DL chamber in the hybrid spherical silica gel prilling granulator of CN872128547 number disclosed rotation of patent, reaction generates positive silicic acid.The further polycondensation of this positive silicic acid is also being revolved mixed chamber, and granulation constitutes in nozzle, the spray orifice; Granularity is at the water-setting silica gel of 1～12mm.The reaction formula that wherein positive silicic acid polycondensation forms silicon sol is expressed as:
The polymer of silica sol particle is more poly-bigger, has just formed the hydrogel of silicon.Type B silica gel of the present invention forms in this prilling granulator exactly, and wherein operating pressure is 0.1～0.4MPa, and temperature of reaction is at 10～40 ℃.
Key point of the present invention is: the water-setting silica gel of making (also claiming virgin rubber, hereinafter to be referred as virgin rubber) is carried out a series of aftertreatment technologys, just can make the Type B silica gel of the object of the invention defined.These aftertreatment technologys have:
(1) burin-in process: the many grains of the virgin rubber of granulating and forming are inserted in the basic solution, soaked all former micelles 1～10 hour, control alkali lye pH value 8～12,30～80 ℃ of temperature.This technology pH value and temperature in hand is particularly important.In pH value 8～12 scopes,, make the SiO of virgin rubber inside owing to the effect of OH base
4The sensible hole of the tridimensional network that tetrahedral structure forms, pore volume is moderate.This is because the OH base can make than the micropore expansion, strengthens the hole geometry of (Si-O-Si) key wall, makes the three-dimensional netted hole of virgin rubber moderate.
(2) acidification:, insert acidic solution again and soaked 1～8 hour with above-mentioned all former micelles.The compound concentration of this acidic solution should be at 1.5～3.5% (w/v).This technology, the first step purpose are the effects that stops the OH base, and the second step purpose is and then uses H
+Effect virgin rubber surfaces externally and internally, thus the Na that is adsorbed on its face replaced
+Deng metal ion.Because H
+The ionic effect makes how much pore texture typings of virgin rubber inside.According to the pH value that former process is handled, temperature, the time, the corresponding processing condition of determining this acidification make this procedure produce the integrated complementary effect, to keep the hole geometry moderate.
(3) washing is handled: with above-mentioned all former micelles, the tap water with clean keeps certain temperature: 20～70 ℃, wash 2～10 times, and washed 3 hours at every turn.This technology utilization warm water is with Na in the virgin rubber
+Deng metal ion H
+Ion SO
4 -Flushings such as ion are removed, and are washed till till the wash water pH value 7, for next step activating process is laid a solid foundation.
(4) tensio-active agent is handled: with above-mentioned all former micelles, insert content again in the nonionic surfactant solution of 1～8% (w/v), immersion treatment 1～12 hour.The key of this technology is, adopts and leaves standstill immersion, makes active agent molecule from outward appearance to inner essence infiltrate virgin rubber hole surfaces externally and internally, thereby can reduce the tension force of virgin rubber pore surface.Like this when next procedure " drying "; because the hot flash evaporation of chance of moisture; and pore surface prestress suddenly increased phenomenon inside and outside virgin rubber can take place, and at this moment can slow down prestressed increase owing to the shielding effect of tensio-active agent, thus the relative rigid matrix structure of protection silica gel.Through activation treatment silica gel, at preparation fragrance silica gel, when inserting silica gel in the spice solution, the unlikely chance water of this silica gel hurriedly bursts, so this silica gel can be used as the raw material of fragrance silica gel.
The selected nonionic surface active agent of the present invention can be: sim alkylphenol Soxylat A 25-7 (TX-9), aliphatic alcohol polyethenoxy silane ether (WA), aliphatic alcohol polyethenoxy thioether, fatty acid amide polyoxyethylene, silk impregnating agent M, the green FB of mill base, poly-ethanol etc.One or more be selected to systems in these nonionogenic tensides are joined the solution of 41-8%.
(5) drying treatment: the former micelle that above-mentioned four step process are handled, in the pallet of packing into, in drying shed, through the oven dry 48 hours down of 80～150 ℃ of hot blasts, after sieving and grading, packaging final prod.
Because virgin rubber is carried out above-mentioned art breading, each treatment process condition is replenished synergy mutually, and make the product of producing and manufacturing technique of the present invention reach: mean pore size is at 0.004～0.007 μ, and average specific surface area is at 400～700m
2/ g, mean particle size is at 1～8mm, and the adsorptive capacity of silica gel is at (60～80) % under relative humidity 90% situation.
Embodiments of the invention are as follows, and protection scope of the present invention is not limited only among the embodiment.
In the experiment, the prepare silicon acid sodium solution reaches 24.5Beo and makes virgin rubber through nozzle in the CN872128547 patent equipment, its reaction formula with 20% sulphuric acid soln that is mixed with:
The processing condition of drying treatment: the virgin rubber of above-mentioned each batch number, shakeout the 30mm thick-layer in baking chamber (case) through sabot, the hot-air seasoning temperature is 120 ℃ ± 5 ℃, the scholar is to silica gel water content≤2% in baking.Analytical test sees Table 2.
Table 2:
Table 1
Claims (3)
1. the producing and manufacturing technique of a Type B silica gel, at first reaction in the hybrid spherical silica gel prilling granulator of rotation generates positive silicic acid by sodium silicate aqueous solution and dilution heat of sulfuric acid for it, and then in, the nozzle indoor in DL step by step polycondensation be a granulated into water-setting silica gel (hereinafter to be referred as: virgin rubber), this device operating pressure is: 0.1～0.4MPa, and temperature of reaction exists: 10～40 ℃; It is characterized in that: the aftertreatment technology to all former micelles is,
(1) burin-in process: with the many former micelle of granulating and forming, insert in the basic solvent, soaked 1～10 hour, control alkali lye pH value 8～12,30～80 ℃ of temperature,
(2) acidification: with above-mentioned all former micelles, insert in the acid solvent again, soaked 1～8 hour, wherein the compound concentration of acidic solution is at 1.5～3.5% (w/v),
(3) washing is handled: wash above-mentioned all former micelles with clean tap water, keep water temperature, wash 2～10 times, washed 3 hours at every turn, be washed till till the pH value 7 at 20～70 ℃,
(4) tensio-active agent is handled: with above-mentioned all former micelles, insert content again in the nonionic surface active agent solvent of 1～8% (w/v), immersion treatment 1～12 hour;
(5) drying treatment: all former micelle that above-mentioned four steps are handled, through hot wind drying room hot-air seasoning 48 hours, wherein hot blast temperature was at 80～150 ℃.
2. producing and manufacturing technique according to claim 1, it is characterized in that: described nonionic surface active agent can be selected for use: the sim alkylphenol Soxylat A 25-7, aliphatic alcohol polyethenoxy silane ether, the aliphatic alcohol polyethenoxy thioether, the fatty acid amide polyoxyethylene, silk impregnating agent M, the green FB polyoxyethylene glycol of mill base, wherein optional one or more systems are joined solution and are used it.
3. producing and manufacturing technique according to claim 1 and the Type B silica gel product made, it is characterized in that: the mean pore size of this silica gel is at 0.004～0.007 μ, and average specific surface area is at 400～700m
2/ g, under relative humidity 90% situation, its adsorptive capacity is 70～80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93110232 CN1031749C (en) | 1993-01-04 | 1993-01-04 | Production process of silica gel and silica gel product thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93110232 CN1031749C (en) | 1993-01-04 | 1993-01-04 | Production process of silica gel and silica gel product thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1089573A CN1089573A (en) | 1994-07-20 |
| CN1031749C true CN1031749C (en) | 1996-05-08 |
Family
ID=4988123
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93110232 Expired - Fee Related CN1031749C (en) | 1993-01-04 | 1993-01-04 | Production process of silica gel and silica gel product thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1031749C (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100436316C (en) * | 2005-12-16 | 2008-11-26 | 厦门大学 | Preparation method of silica gel carrier |
| WO2012147002A1 (en) * | 2011-04-29 | 2012-11-01 | Construction Research & Technology Gmbh | Process for producing hydrogels |
| CN109292784B (en) * | 2018-10-25 | 2021-10-01 | 青岛美高集团有限公司 | Preparation method of silica gel and silica gel obtained by preparation method |
| ES2983742T3 (en) * | 2018-12-17 | 2024-10-24 | Taghleef Ind Inc | Printable Movie |
| CN110079217A (en) * | 2019-06-06 | 2019-08-02 | 东莞市富鼎新材料科技有限公司 | A kind of self-lubricating polishing silica gel material and preparation method thereof and product |
-
1993
- 1993-01-04 CN CN 93110232 patent/CN1031749C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1089573A (en) | 1994-07-20 |
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