CN1958447A - Preparation method of high-purity silica gel - Google Patents
Preparation method of high-purity silica gel Download PDFInfo
- Publication number
- CN1958447A CN1958447A CN 200510117271 CN200510117271A CN1958447A CN 1958447 A CN1958447 A CN 1958447A CN 200510117271 CN200510117271 CN 200510117271 CN 200510117271 A CN200510117271 A CN 200510117271A CN 1958447 A CN1958447 A CN 1958447A
- Authority
- CN
- China
- Prior art keywords
- silica gel
- silicate
- preparation
- acid
- purity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000000741 silica gel Substances 0.000 title claims abstract description 49
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000499 gel Substances 0.000 claims abstract description 18
- 239000012452 mother liquor Substances 0.000 claims abstract description 11
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 150000001768 cations Chemical class 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims description 21
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 12
- 239000011707 mineral Substances 0.000 claims description 12
- 235000019353 potassium silicate Nutrition 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000004111 Potassium silicate Substances 0.000 claims description 3
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 32
- 239000003054 catalyst Substances 0.000 abstract description 8
- 150000007522 mineralic acids Chemical class 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000003729 cation exchange resin Substances 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 229960001866 silicon dioxide Drugs 0.000 description 42
- 238000000034 method Methods 0.000 description 22
- 239000000243 solution Substances 0.000 description 19
- 229910004298 SiO 2 Inorganic materials 0.000 description 17
- 239000002245 particle Substances 0.000 description 9
- 238000000746 purification Methods 0.000 description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004438 BET method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007962 solid dispersion Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000005507 spraying Methods 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention provides a preparation method of high-purity silica gel, which comprises the steps of firstly, enabling a silicate solution to pass through an ion exchange column filled with cation exchange resin for ion exchange, removing cation impurities in the silicate solution, placing a part of purified silicate solution into a reaction kettle with a stirrer, keeping the temperature constant for several hours to form mother liquor, then simultaneously adding the rest silicate solution and inorganic acid into the reaction kettle, carrying out constant-temperature aging on silica gel obtained after reaction, adjusting the pH value, carrying out constant-temperature chambering, washing and drying to obtain the silica gel. The high-purity silica gel has controllable pore volume of 0.6-2.5 ml/g, average pore size distribution of 8-26 nm, bulk density of 0.2-0.5 g/ml, purity of over 99.5%, excellent mechanical performance, and capacity of preparing various catalysts or catalyst carrier silica gels by regulating technological parameters.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity silica gel, can prepare high grade catalyzer or multiple high purity catalyst carrier silica gel by the adjusting process parameter.
Background technology
Silica gel is a kind of porous material, also is important inorganic chemical product.Silica gel is mainly used in sorbent material, siccative, weighting agent, chromatographic grade carrier etc.Development along with oil and petrochemical complex, silica gel is more and more as catalyzer and support of the catalyst, silica gel is because the structure difference of gel skeleton, on performance, show than big difference, traditional preparation of silica gel method is to join reaction generation silicic acid in the water glass with sulfuric acid, the silicic acid instability forms silicon sol by intermolecular condensation, and silicon sol just becomes silica gel through operations such as aging, washing, dryings again behind gel.Patent CN1158310 directly gets the part silicate solutions to prepare nucleus, again with silicate solutions directly with the method for preparing silica gel of inorganic acid reaction generation gel, obtained silica gel purity, pore volume, aperture are limited, can only be used for olefinic polyreaction as metallocene catalysis agent carrier silica gel special.CN103822A improves the silica gel aperture by the solution pressurized heat is handled.Patent CN0215935518 places the basic solution heat drying to make the technology of wide aperture silica gel in small-bore silica gel.CN1081608C is a kind of preparation of silica gel method of adjusting porous structure, this method adopts after tradition " forming oil column " the device preparation hydrogel, use tensio-active agent as aging medium, make silica gel through aging, dry, roast, its mean pore size is at 0.004~0.015 μ m, and specific surface is at 80~500m
2/ g, pore volume is at 0.3~1.2ml/g.
Patent CN1157260A discloses alkaline silica gel acid solution and mineral acid, by an instantaneous mixing of second fluid nozzle, the colloidal sol that forms is discharged in the solvent that is dissolved with gas and is formed gel, it is characterized in that using the water-insoluble solid dispersion agent, join alkaline silicate solution or mineral acid at least a among, can enlarge markedly the aperture of spherical silica-gel.
Summary of the invention
The invention provides a kind of high-purity silica gel preparation method who is suitable for doing catalyzer or support of the catalyst.
The preparation method of high-purity silica gel is as follows:
At first be that 6.0%~18% silicate solutions is by an ion exchange column that Zeo-karb is housed with concentration, carry out ion-exchange, remove the cation impurity in the silicate solutions, (1/1.5)~(1/15) silicate solutions of the silicate solutions gross weight behind the purifying is inserted in the reactor of band stirring, 20~90 ℃ of following constant temperature 0.5~3.0 hour, be preferably at 40~80 ℃ of following constant temperature and formed mother liquor in 0.5~2.0 hour, joined remaining silicate solutions and mineral acid in the reactor simultaneously with 0.5~3.0 hour again, the silicon gel of gained is aging through 0.5~3.0 hour constant temperature, PH is transferred to 2.0~8.5, carried out reaming in 2.0~8.0 hours through 40~80 ℃ of following constant temperature again, washing, dry, promptly obtain silica gel of the present invention, purity can reach more than 99%.Washing, drying can adopt usual way to carry out, and the present invention is not limited, and drying preferably adopts spraying drying.
Mesosilicic acid salts solution of the present invention must pass through purification process, and cation impurity is meant cation impurities such as Na, Ca, Fe.After the process strongly acidic cation-exchange carries out ion exchange treatment, be particularly suitable for getting the part silicate solutions and prepare nucleus, again with silicate solutions directly with the method for preparing silica gel of inorganic acid reaction generation gel, it has not only improved the purity of product silica gel, and can also form closely knit nucleus, make silica gel have good mechanical property (resistance to wearing) as the intensity height, by the adjusting process parameter, other rerum natura brand silica gel of easier acquisition, make silica gel more wide, have the unexistent excellent effect of other method in Application Areas.
Silicate solutions can be a kind of, also can be the mixture of multiple silicate, and as being water glass, potassium silicate, Starso etc., the mineral acid of adding can be sulfuric acid, nitric acid, hydrochloric acid or mixing acid.The add-on of mineral acid is the general add-on that adopts when being raw material production silica gel with silicate, and the mol ratio of silicate and mineral acid is (1: 0.65)~(1: 1.38), and preferable mol ratio is (1: 0.75)~(1: 1.16).
SiO
2The growth of particle is carried out according to piling up theory, at first will form SiO
2Nucleus, silicate solutions SiO usually
2Be with single silicic acid [Si (OH)
4] the formation existence, single silicic acid Si (OH)
4At suitable surface charge, SiO
2Polycondensation mutually under the conditions such as concentration, temperature, pH value forms SiO
2Nucleus.The present invention is with silicate solutions system mother liquor behind the partial purification, the temperature, the SiO that are being fit to
2Under the conditions such as concentration, just can form closely knit active SiO
2Nucleus.By adding silicate solutions and mineral acid, can make single silicic acid Si (OH)
4Form the monomer particle, along with the increase of monomer particle concentration, high density monomer particle forms dissolution equilibrium, and the SiO that is deposited in the growth is dissolved in the depolymerization of oligopolymer
2On the nucleus, by regulating the adding speed of back adding purifying silicon acid salt solution and the molten ratio of rolling of mother liquor silicate and temperature of reaction and silicate solutions, size and the particle distribution that can regulate particle diameter.
Use technology of the present invention to be particularly useful for making and require very high catalyzer of purity or support of the catalyst silica gel.
The high-purity silica gel SiO of the technology of the present invention preparation
2Content the best can be greater than 99.5%, and specific surface can be at 200~500m
2Regulate SiO in the colloidal sol scope in the/g
2The size of particle diameter has directly determined the specific surface value of final silica gel, according to derive rough and ready formula: S=3000/D wherein S be specific surface area (m
2/ g), D is primary particle size diameter (nm).Primary particle size is controlled at 6~15nm, in order to realize colloidal sol SiO
2Particle can be at 6~15nm, and the mother liquor amount in early stage will be controlled in (1/1.5)~(1/15) of total amount, reinforced 0.5~3.0 hour time.The mother liquor amount in early stage is greater than 1/1.5 when above of total amount, and the specific surface of silica gel is greater than 500m
2/ g; The reinforced time, too short meeting formed new nucleus, caused the silica gel particle diameter inhomogeneous, and reinforced overlong time influences the throughput of silica gel device.
High-purity silica gel preparation method provided by the invention, its characteristics are at first with raw silicon acid salt solution purifying, according to piling up theory with this silicate solutions and mineral acid effect, prepare high-purity silica gel, this product can be used for exigent catalyzer or multiple high-purity support of the catalyst.By the high-purity silica gel that the inventive method is made, can be by regulating pH value control pore volume at 0.6~2.5ml/g, mean pore size is distributed in 8~26nm.Bulk density can prepare multiple catalyzer or support of the catalyst silica gel at 0.2~0.5g/ml by the adjusting process parameter.
Embodiment
Raw material sources:
Ion exchange resin a: Zeo-karb of strong acid (Shanghai Resin Factory)
Analytical procedure:
SiO
2Content: atomic absorption spectrum is surveyed silica gel impurity method
Specific surface: BET method (specific surface and pore analysis instrument fast)
Pore volume: BJH method
Bulk density: GB 7823-87
Mean pore size: BET method (specific surface and pore analysis instrument fast)
Wear rate: (intensity friabilator)
Embodiment 1
At first be that 15% rare water glass carries out ion-exchange by an ion exchange column that a Zeo-karb of strong acid is housed with 1000ml concentration, remove the Na in the water glass, Ca, the Fe plasma, get 200ml and put into reactor, stir maintenance 1 hour down at 50 ℃, join in the reactor simultaneously with 1.5 hours analytical pure sulfuric acids again with water glass behind the remaining 800ml purifying and 270ml 10%, after silicic acid all is converted into gel, constant temperature wore out in 2.0 hours, pH is transferred to 6.0, temperature was carried out reaming in 7 hours at 80 ℃ of following constant temperature, with drying 10 hours at 100~120 ℃ behind the distilled water wash, promptly get the high-purity silica gel of preparation of the present invention.Test result is: SiO
2Content 99.6%, specific surface 287m
2/ g, pore volume 1.88ml/g, bulk density 0.25g/ml, mean pore size
Wear rate is 8.2%.
Embodiment 2
The purification process of silicate and preparing gel and post-treating method are fully with embodiment 1, but rare Starso of raw material employing 15% and rare potassium silicate of 20%, by volume 1.5: 1 mixed mixed silicates.Silica gel records the result and is SiO
2Content 99.56%, specific surface 306m
2/ g, pore volume 1.82ml/g, bulk density 0.27g/ml, mean pore size
Wear rate is 8.3%.
Embodiment 3
The purification process of silicate and preparing gel and post-treating method be fully with embodiment 1, and used inorganic salt adopt the dilute hydrochloric acid by volume 2: 1 of 10% dilute sulphuric acid and 10% as mixing acid.The silica gel test result is: SiO
2Content 99.58%, specific surface 260m
2/ g, pore volume 1.83ml/g, bulk density 0.265g/ml, mean pore size
Wear rate is 8.3%.
Embodiment 4
Silicate purifying, preparing gel and post-treating method be fully with embodiment 1, and the dilute silicate of getting behind the 600ml purifying is put into reactor, and the mother liquor amount is increased to 600ml by the 200ml of embodiment 1, and test result is: SiO
2Content 99.55%, specific surface 476m
2/ g, pore volume 1.22ml/g, bulk density 0.298g/ml, mean pore size
Wear rate is 8.35%.
Embodiment 5
The purification process of silicate and preparing gel and post-treating method transfer to 3.0 with pH after wearing out and carry out reaming fully with embodiment 1.Test result is: SiO
2Content 99.52%, specific surface 299m
2/ g, pore volume 0.72ml/g, bulk density 0.286g/ml, mean pore size
Wear rate is 8.25%.
Embodiment 6
The purification process of silicate and preparing gel and post-treating method just rise to 65 ℃ with the mother liquor preparation temperature by 50 ℃ fully with embodiment 1, and experimental result is: SiO
2Content 99.55%, specific surface 202m
2/ g, pore volume 1.52ml/g, bulk density 0.298g/ml, mean pore size
Wear rate is 8.32%.
Embodiment 7
The purification process of silicate and preparing gel and post-treating method carried out reaming in 7 hours with 80 ℃ of constant temperature and change the reaming in 3 hours of 60 ℃ of constant temperature into fully with embodiment 1, and experimental result is: SiO
2Content 99.6%, specific surface 267m
2/ g, pore volume 1.34ml/g, bulk density 0.25g/ml, mean pore size
Wear rate is 8.22%.
Comparative Examples 1
Preparing gel and post-treating method are fully with embodiment 1, but the raw silicon hydrochlorate does not carry out passivation, and experimental result is: SiO
2Content 98.28%, specific surface 316m
2/ g, pore volume 1.56ml/g, bulk density 0.28/ml, mean pore size
Wear rate is 18.6%.
Comparative Examples 2
The purification process of silicate and preparing gel and post-treating method are fully with embodiment 1, but the mother liquor amount changes 800ml into by 200ml, and experimental result is: SiO
2Content 99.6%, specific surface 615m
2/ g, pore volume 0.96ml/g, bulk density 0.36g/ml, mean pore size
Wear rate is 8.1%.
Comparative Examples 3
The purification process of silicate and preparing gel and post-treating method transfer to 1.0 with pH after wearing out and carry out reaming fully with embodiment 1.Test result is: SiO
2Content 99.52%, specific surface 338m
2/ g, pore volume O.5lml/g, bulk density O.359g/ml, mean pore size
Wear rate is 8.22%.
Claims (6)
1. the preparation method of a high-purity silica gel, at first be that 6.0%~18% silicate solutions is by an ion exchange column that Zeo-karb is housed with concentration, carry out ion-exchange, remove the cation impurity in the silicate solutions, (1/1.5)~(1/15) silicate solutions of the silicate solutions gross weight behind the purifying is inserted in the reactor of band stirring, formed mother liquor in 0.5~3.0 hour at 20~90 ℃ of following constant temperature, joined remaining silicate solutions and mineral acid in the reactor simultaneously with 0.5~3.0 hour again, the silicon gel of reaction back gained is aging through 0.5~3.0 hour constant temperature, PH is transferred to 2.0~8.5, carried out reaming in 2.0~8.0 hours through 40~80 ℃ of following constant temperature again, washing, drying promptly obtains silica gel.
2. preparation method according to claim 1 is characterized in that forming mother liquor in 0.5~2.0 hour at 40~80 ℃ of following constant temperature.
3. preparation method according to claim 1 is characterized in that mineral acid is sulfuric acid, nitric acid, hydrochloric acid or their mixing acid.
4. preparation method according to claim 1 is characterized in that silicate is one or more in water glass, potassium silicate, the Starso.
5. preparation method according to claim 1 is characterized in that the mol ratio of silicate and mineral acid is (1: 0.65)~(1: 1.38).
6. preparation method according to claim 1 is characterized in that the mol ratio of silicate and mineral acid is (1: 0.75)~(1: 1.16).
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2005101172716A CN100443406C (en) | 2005-11-03 | 2005-11-03 | Preparation method of high-purity silica gel |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2005101172716A CN100443406C (en) | 2005-11-03 | 2005-11-03 | Preparation method of high-purity silica gel |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1958447A true CN1958447A (en) | 2007-05-09 |
CN100443406C CN100443406C (en) | 2008-12-17 |
Family
ID=38070318
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2005101172716A Active CN100443406C (en) | 2005-11-03 | 2005-11-03 | Preparation method of high-purity silica gel |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100443406C (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102649091A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Preparation method of catalyst carrier used in hydrogenation production of ethylene glycol from oxalate |
CN103954618A (en) * | 2014-04-23 | 2014-07-30 | 叶伟荣 | Method for determining concentration of glucose by using colorimetric method |
CN105289466A (en) * | 2015-12-11 | 2016-02-03 | 中国海洋石油总公司 | Absorbent for absorbing and separating polyaromatic hydrocarbon in diesel and preparation method thereof |
CN114229850A (en) * | 2021-12-17 | 2022-03-25 | 厦门世达膜科技有限公司 | Production method for converting sodium silicate into silicic acid |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1158310C (en) * | 2001-09-03 | 2004-07-21 | 中国石油天然气股份有限公司 | Preparation method of silica gel carrier |
CN1260125C (en) * | 2004-04-09 | 2006-06-21 | 苏州天马医药集团精细化学品有限公司 | Method for fabricating nano sol of silicon dioxide in use for papermaking |
-
2005
- 2005-11-03 CN CNB2005101172716A patent/CN100443406C/en active Active
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102649091A (en) * | 2011-02-25 | 2012-08-29 | 中国石油化工股份有限公司 | Preparation method of catalyst carrier used in hydrogenation production of ethylene glycol from oxalate |
CN103954618A (en) * | 2014-04-23 | 2014-07-30 | 叶伟荣 | Method for determining concentration of glucose by using colorimetric method |
CN105289466A (en) * | 2015-12-11 | 2016-02-03 | 中国海洋石油总公司 | Absorbent for absorbing and separating polyaromatic hydrocarbon in diesel and preparation method thereof |
CN114229850A (en) * | 2021-12-17 | 2022-03-25 | 厦门世达膜科技有限公司 | Production method for converting sodium silicate into silicic acid |
Also Published As
Publication number | Publication date |
---|---|
CN100443406C (en) | 2008-12-17 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Jusoh et al. | Sequential desilication–isomorphous substitution route to prepare mesostructured silica nanoparticles loaded with ZnO and their photocatalytic activity | |
JP4478766B2 (en) | Spherical silica porous particles and method for producing the same | |
CN103265050B (en) | A kind of method preparing multi-stage pore zeolite molecular sieve microsphere | |
JPS63162521A (en) | Novel synthesis of ferric silicate type zeolites, obtained substances and their uses | |
CN101468318B (en) | Modified rare-earth-containing molecular sieve catalyst as well as preparation method and use thereof | |
KR20090022664A (en) | Production and use of polysilicate particulate materials | |
CN100431965C (en) | Round alumina of containing silicon, and preparation method | |
CN103508463B (en) | Preparation method of binderless spherical faujasite particles | |
CN104229818B (en) | Synthesis method of beta molecular sieve | |
KR20140063709A (en) | Methods for forming zeolites from homogeneous amorphous silica alumina | |
CN100443406C (en) | Preparation method of high-purity silica gel | |
CN103318910A (en) | Method for preparing large-size analcite by utilizing hydrothermal crystallization of geopolymer | |
CN101973557B (en) | Method for preparing high-purity mono-disperse silicon dioxide hydrosol | |
CN106622378A (en) | Spherical aluminium-containing mesoporous composite material, supported catalyst, preparation method and applications of spherical aluminium-containing mesoporous composite material and supported catalyst, and method used for preparing cyclohexanone glyceryl | |
CN109718826B (en) | Microsphere Silicate-1 molecular sieve catalyst, preparation method thereof and method for preparing caprolactam | |
US20060099130A1 (en) | Silica mesoporous materials | |
US7097772B2 (en) | Method of purifying a waste stream using a microporous composition | |
CN107840349A (en) | The preparation method of the nanometer multi-stage porous aggregations of ZSM 5 | |
CN115231595A (en) | Preparation method of pseudo-boehmite with high specific surface area | |
CN109046341A (en) | A kind of preparation method of visible light-responded silver silicate/concave convex rod composite catalyst | |
CN110228812A (en) | A kind of binderless A type sieve particle and preparation method thereof | |
CN110172158B (en) | Preparation method of hierarchical porous metal organic framework material MIL-101(Cr) | |
CN104549460B (en) | Composite molecular sieve, as well as preparation method and application thereof | |
CN103435063B (en) | Preparation method of amorphous nano SiO2/A zeolite composite powder | |
CN101195490B (en) | Method for producing middle and fine diplopore molecular sieve with nano-minicrystal and ionic surface active agent in microwave radiation condition |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant |