CN104923301A - High-temperature-resistant cryolite-based composite solid acid catalyst and preparation method therefor - Google Patents
High-temperature-resistant cryolite-based composite solid acid catalyst and preparation method therefor Download PDFInfo
- Publication number
- CN104923301A CN104923301A CN201510241703.8A CN201510241703A CN104923301A CN 104923301 A CN104923301 A CN 104923301A CN 201510241703 A CN201510241703 A CN 201510241703A CN 104923301 A CN104923301 A CN 104923301A
- Authority
- CN
- China
- Prior art keywords
- parts
- acid catalyst
- cryolite
- composite solid
- resistant
- 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.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 239000011973 solid acid Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910001610 cryolite Inorganic materials 0.000 title abstract 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004743 Polypropylene Substances 0.000 claims abstract description 9
- 239000000835 fiber Substances 0.000 claims abstract description 9
- -1 polypropylene Polymers 0.000 claims abstract description 9
- 229920001155 polypropylene Polymers 0.000 claims abstract description 9
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 9
- 239000000661 sodium alginate Substances 0.000 claims abstract description 9
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920002545 silicone oil Polymers 0.000 claims abstract description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 7
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010335 hydrothermal treatment Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 abstract description 5
- 229910003849 O-Si Inorganic materials 0.000 abstract description 4
- 229910003872 O—Si Inorganic materials 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000003377 acid catalyst Substances 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 238000011068 loading method Methods 0.000 abstract description 2
- 230000020477 pH reduction Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 3
- 239000011324 bead Substances 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- JHUUPUMBZGWODW-UHFFFAOYSA-N 3,6-dihydro-1,2-dioxine Chemical compound C1OOCC=C1 JHUUPUMBZGWODW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Landscapes
- Catalysts (AREA)
Abstract
The invention discloses a high-temperature-resistant cryolite-based composite solid acid catalyst and a preparation method therefor. The high-temperature-resistant cryolite-based composite solid acid catalyst is characterized by being prepared from the following raw materials in parts by weight: 41-52 parts of gamma-alumina, 5-8 parts of cryolite, 9-14 parts of hollow glass beads, 26-38 parts of silicon dioxide, 11-15 parts of polypropylene fibers, 1-2 parts of aluminum chloride, 2-4 parts of sodium alginate, 13-17 parts of vinyl silicone oil and a proper amount of water. According to the high-temperature-resistant cryolite-based composite solid acid catalyst, an aqueous solution of aluminum chloride and sodium alginate is uniformly loaded on silicon dioxide after carrying out acidification treatment on a cryolite surface so as to form a stable Al-O-Si and Na-O-Si covalent structure; the structure of the SiO2 is not damaged by the loading process, and the specific surface area of generated complex is relatively large; added polypropylene fiber particles are bonded on the surface of alumina, so that capacity of absorbing H<+> is improved; and compared with a conventional liquid acid catalyst, the high-temperature-resistant cryolite-based composite solid acid catalyst has the advantages of being low in pollution, resistant to high temperature, low in corrosion, liable to recycle, and the like, meets the energy-saving and emission-reducing needs, and is a development direction of a future catalyst.
Description
Technical field
The present invention relates to solid acid catalyst technical field, be specifically related to a kind of high temperature resistant ice crystal ground mass composite solid-acid catalyst and preparation method thereof.
Background technology
Isosorbide-5-Nitrae-dioxane (Isosorbide-5-Nitrae-dioxane), molecular formula C
4h
8o
2, colourless liquid, slightly fragrance, density 1.0329, refractive index 1.4175, fusing point 11 DEG C, boiling point 101.1 DEG C, with water and many immiscible organic solvents, be the solvent of cellulose acetate, resin, vegetable oil, mineral oil, oil-soluble dyes etc., also for system spray paint, varnish, plasticizer, wetting agent etc.
1 is produced at present in the chemical production processes of reality, 4-dioxane great majority still adopt liquid acid such as the concentrated sulfuric acid as catalyst, although have inexpensive, reaction temperature is low, conversion ratio is high, reactivity advantages of higher, but there is, raffinate serious to equipment corrosion and waste water environmental pollution is serious, operating condition is harsh, product post processing is more difficult, accessory substance is many, poor selectivity and be difficult to realize the shortcomings such as continuous seepage in technique, the needs of current environmental protection and economic development can not be met; Though existing fraction enterprise adopts solid acid catalyst aluminium oxide or molecular sieve etc. in prior art, exist be easy to solution-off, less stable, life-span compared with short, easy in inactivation, the defect such as acid strength distribution is wide, aperture is little, the surface nature of easy carbon distribution, catalyst is complicated.If prepare nontoxic composite solid-acid catalyst, then above-mentioned problems just can be resolved, and replace liquid acid as catalyst to be also the important channel realizing environmental friendly catalysis new technology with solid acid.
Summary of the invention
Object of the present invention is just to provide a kind of high temperature resistant ice crystal ground mass composite solid-acid catalyst and preparation method thereof, to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this:
A kind of high temperature resistant ice crystal ground mass composite solid-acid catalyst, it is characterized in that, be made up of the raw material of following weight portion: gama-alumina 41-52, ice crystal 5-8, hollow glass micropearl 9-14, silica 26-38, polypropylene fiber 11-15, aluminium chloride 1-2, sodium alginate 2-4, vinyl silicone oil 13-17, suitable quantity of water.
The preparation method of described a kind of high temperature resistant ice crystal ground mass composite solid-acid catalyst, is characterized in that comprising the following steps:
(1) aluminium chloride, sodium alginate are added water to be stirred to and dissolve completely, add ice crystal and soak 10-12 hour, grinding pulping, add silica and flood absorption 2-4 hour under high velocity agitation, be placed in stainless steel cauldron, in 110 DEG C of hydrothermal treatment consists 6h after sealing, suction filtration, washing, dry at 80 DEG C, grind for subsequent use;
(2) polypropylene fiber is crushed to 200-300 order, adds gama-alumina, vinyl silicone oil ultrasonic wave is dried for dispersion grinding 3-5 hour;
(3) by step (1), the mixing of (2) material, add other residual components and stir 30-50 minute, microwave drying grinding discharging in 3 hours at leaving standstill 1-5 hour, 160-180 DEG C.
The present invention has following beneficial effect: the present invention adopts aluminium chloride, sodium alginate aqueous solution, and to after the acidification of ice crystal surface, uniform load is on silica, and form the covalent structure of stable Al-O-Si and Na-O-Si, loading process does not destroy SiO
2structure and the compound specific area generated is comparatively large, add polypropylene fiber particles stick at alumina surface simultaneously, improve absorption H
+ability, obtained composite solid-acid catalyst has low stain, high temperature resistant, low corrosion compared to traditional liquid acid catalyst and is easy to the advantages such as recovery, and meeting the requirement of energy-saving and emission-reduction, is the developing direction of following catalyst.
Detailed description of the invention
Described one is high temperature resistant ice crystal ground mass composite solid-acid catalyst, it is characterized in that, be made up of the raw material of following weight portion: gama-alumina 46, ice crystal 6, hollow glass micropearl 11, silica 28, polypropylene fiber 14, aluminium chloride 2, sodium alginate 4, vinyl silicone oil 15, suitable quantity of water.
Preparation method comprises the following steps:
(1) aluminium chloride, sodium alginate are added water to be stirred to and dissolve completely, add ice crystal and soak 10-12 hour, grinding pulping, add silica and flood absorption 2-4 hour under high velocity agitation, be placed in stainless steel cauldron, in 110 DEG C of hydrothermal treatment consists 6h after sealing, suction filtration, washing, dry at 80 DEG C, grind for subsequent use;
(2) polypropylene fiber is crushed to 200-300 order, adds gama-alumina, vinyl silicone oil ultrasonic wave is dried for dispersion grinding 3-5 hour;
(3) by step (1), the mixing of (2) material, add other residual components and stir 30-50 minute, microwave drying grinding discharging in 3 hours at leaving standstill 1-5 hour, 160-180 DEG C.
The technical parameter index of the composite solid-acid catalyst using the present invention to produce is as follows: catalytic production Isosorbide-5-Nitrae-dioxane conversion ratio is 65.73%, selective close to 100%.
Claims (2)
1. a high temperature resistant ice crystal ground mass composite solid-acid catalyst, it is characterized in that, be made up of the raw material of following weight portion: gama-alumina 41-52, ice crystal 5-8, hollow glass micropearl 9-14, silica 26-38, polypropylene fiber 11-15, aluminium chloride 1-2, sodium alginate 2-4, vinyl silicone oil 13-17, suitable quantity of water.
2. the preparation method of a kind of high temperature resistant ice crystal ground mass composite solid-acid catalyst according to claim 1, is characterized in that comprising the following steps:
(1) aluminium chloride, sodium alginate are added water to be stirred to and dissolve completely, add ice crystal and soak 10-12 hour, grinding pulping, add silica and flood absorption 2-4 hour under high velocity agitation, be placed in stainless steel cauldron, in 110 DEG C of hydrothermal treatment consists 6h after sealing, suction filtration, washing, dry at 80 DEG C, grind for subsequent use;
(2) polypropylene fiber is crushed to 200-300 order, adds gama-alumina, vinyl silicone oil ultrasonic wave is dried for dispersion grinding 3-5 hour;
(3) by step (1), the mixing of (2) material, add other residual components and stir 30-50 minute, microwave drying grinding discharging in 3 hours at leaving standstill 1-5 hour, 160-180 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510241703.8A CN104923301A (en) | 2015-05-13 | 2015-05-13 | High-temperature-resistant cryolite-based composite solid acid catalyst and preparation method therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510241703.8A CN104923301A (en) | 2015-05-13 | 2015-05-13 | High-temperature-resistant cryolite-based composite solid acid catalyst and preparation method therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104923301A true CN104923301A (en) | 2015-09-23 |
Family
ID=54110913
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510241703.8A Pending CN104923301A (en) | 2015-05-13 | 2015-05-13 | High-temperature-resistant cryolite-based composite solid acid catalyst and preparation method therefor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104923301A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116656190A (en) * | 2022-12-31 | 2023-08-29 | 苏州弗克技术股份有限公司 | Interface coating for monocomponent vitreous substrate and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4415480A (en) * | 1981-09-24 | 1983-11-15 | Exxon Research And Engineering Co. | Transition metal oxide Bronsted acid catalysts |
| CN1649186A (en) * | 2004-01-05 | 2005-08-03 | 现代自动车株式会社 | Solid oxide fuel cell sealant comprising glass matrix and ceramic fiber and method of manufacturing the same |
| CN1858160A (en) * | 2006-06-02 | 2006-11-08 | 中国农业科学院油料作物研究所 | Method for preparing biological diesel oil using nano solid acid or alkali catalyst |
| CN101125791A (en) * | 2007-08-06 | 2008-02-20 | 大连理工大学 | A new method to make adamantane on solid acid catalyst |
| CN103242270A (en) * | 2013-05-28 | 2013-08-14 | 华东理工大学 | Method for preparing furfural compounds from biomass |
| CN103691463A (en) * | 2013-12-17 | 2014-04-02 | 中国科学院长春应用化学研究所 | Solid acid catalyst and preparation method thereof, and preparation method of diolefin compounds |
-
2015
- 2015-05-13 CN CN201510241703.8A patent/CN104923301A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4415480A (en) * | 1981-09-24 | 1983-11-15 | Exxon Research And Engineering Co. | Transition metal oxide Bronsted acid catalysts |
| CN1649186A (en) * | 2004-01-05 | 2005-08-03 | 现代自动车株式会社 | Solid oxide fuel cell sealant comprising glass matrix and ceramic fiber and method of manufacturing the same |
| CN1858160A (en) * | 2006-06-02 | 2006-11-08 | 中国农业科学院油料作物研究所 | Method for preparing biological diesel oil using nano solid acid or alkali catalyst |
| CN101125791A (en) * | 2007-08-06 | 2008-02-20 | 大连理工大学 | A new method to make adamantane on solid acid catalyst |
| CN103242270A (en) * | 2013-05-28 | 2013-08-14 | 华东理工大学 | Method for preparing furfural compounds from biomass |
| CN103691463A (en) * | 2013-12-17 | 2014-04-02 | 中国科学院长春应用化学研究所 | Solid acid catalyst and preparation method thereof, and preparation method of diolefin compounds |
Non-Patent Citations (2)
| Title |
|---|
| 王延吉等著: "《绿色催化过程与工艺》", 28 February 2002 * |
| 田部浩三等著: "《新固体酸和碱及其催化作用》", 30 November 1992 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116656190A (en) * | 2022-12-31 | 2023-08-29 | 苏州弗克技术股份有限公司 | Interface coating for monocomponent vitreous substrate and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101830474B (en) | Method for preparing white carbon black | |
| CN102631930A (en) | Catalyst for preparing furfuryl alcohol from furfural by vapor phase hydrogenation and preparation method thereof | |
| CN108722422A (en) | A kind of method of red mud activation modification and application | |
| CN108893031A (en) | A kind of surfacecti proteon coating of anti-seawater corrosion and preparation method thereof | |
| CN101205066A (en) | Macroporous microsphere silica gel and preparation thereof | |
| CN106868948A (en) | A kind of filter paper and its simple method for preparing and application with oil-water separating function | |
| CN104923301A (en) | High-temperature-resistant cryolite-based composite solid acid catalyst and preparation method therefor | |
| CN109734722B (en) | A kind of method for preparing isosorbide by dehydration of sorbitol | |
| CN106748665B (en) | The method of CaO-SBA-15 molecular sieve catalytic makrolon material Methanolysis recycling bisphenol-A | |
| CN102614919A (en) | Sulfonated cross-linked chitosan resin type solid acid catalyst and preparation method thereof | |
| CN101830820B (en) | Method for preparing 2,5-diparamethylaniline terephthalic acid (DTTA) | |
| CN104888761A (en) | Modified silicon dioxide-aluminium oxide composite solid acid catalyst and preparation method thereof | |
| CN104923265A (en) | Recyclable compound solid acid catalyst and preparation method therefor | |
| CN105085335A (en) | Method for preparing 3-mercapto-propionate | |
| CN109233281A (en) | A kind of preparation method of alkalinity quaternary amine PS membrane | |
| CN104923266A (en) | Complex solid acid catalyst suitable for synthesizing ethyl ether by ethanol dehydration and preparation method therefor | |
| CN104874426A (en) | Modified crushed-gravel-based compound solid acid catalyst and preparation method thereof | |
| CN104857992A (en) | Complex solid acid catalyst with high catalytic efficiency and preparation method thereof | |
| CN106966898A (en) | A kind of method that presence of acidic ionic liquid catalyst synthesizes dipropylene glycol methyl ether acetate | |
| CN104923307A (en) | Low-energy consumption non-corrosive compound solid acid catalyst and preparation method therefor | |
| CN104857991A (en) | Nickel sulfate/silicon dioxide composite solid acid catalyst and manufacturing method thereof | |
| CN102260359A (en) | Method for preparing chromium silica gel catalyst carrier with high specific surface area and large pore volume | |
| CN104923311A (en) | High-adsorption complex solid acid catalyst and preparation method therefor | |
| CN104923280A (en) | Compound solid acid catalyst with high nitrate conversion rate and preparation method thereof | |
| CN108031489B (en) | Preparation method and application of fly ash-supported copper p-toluenesulfonate catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150923 |
|
| RJ01 | Rejection of invention patent application after publication |