CN104801327A - Preparation method of solid acid catalyst - Google Patents
Preparation method of solid acid catalyst Download PDFInfo
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- CN104801327A CN104801327A CN201510154308.6A CN201510154308A CN104801327A CN 104801327 A CN104801327 A CN 104801327A CN 201510154308 A CN201510154308 A CN 201510154308A CN 104801327 A CN104801327 A CN 104801327A
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- acid catalyst
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- ammonium
- chloride
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- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- 239000011973 solid acid Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 12
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 12
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000007062 hydrolysis Effects 0.000 claims abstract description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 6
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 6
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 235000014121 butter Nutrition 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000010189 synthetic method Methods 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 13
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 8
- 238000003483 aging Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000002841 Lewis acid Substances 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 150000007517 lewis acids Chemical group 0.000 description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000003930 superacid Substances 0.000 description 4
- 239000003377 acid catalyst Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 229910007926 ZrCl Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003729 cation exchange resin Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical class C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- YZUPZGFPHUVJKC-UHFFFAOYSA-N 1-bromo-2-methoxyethane Chemical compound COCCBr YZUPZGFPHUVJKC-UHFFFAOYSA-N 0.000 description 1
- 238000005727 Friedel-Crafts reaction Methods 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005575 aldol reaction Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 description 1
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 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
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- -1 zeolite molecular sieve class Chemical class 0.000 description 1
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Abstract
The invention particularly provides a preparation method of a solid acid catalyst. The method comprises the following steps: using metal chlorides as raw materials, performing hydrolysis, neutralization, aging, washing and drying, so as to obtain solid powder; fully grinding the solid powder, mixing the ground solid powder with ammonium salt, and roasting, so as to obtain the solid acid catalyst. According to the preparation method of the solid acid catalyst, the raw materials are low in cost and easy to obtain, the synthetic method is simple, and the analysis on a test result shows that the synthesized solid acid catalyst is high in acidity and excellent in heat stability, so that the preparation method has wide application prospect.
Description
Technical field
The invention belongs to chemical reagent synthesis technical field, be specifically related to a kind of preparation method of solid acid catalyst.
Background technology
Acid is the important catalyst of a class, can be used for catalytic esterification, Friedel-Crafts reaction and aldol reaction etc.The acid catalyst of current industrial application is liquid acid catalyst mostly, such as: sulfuric acid, phosphoric acid, nitric acid, hydrochloric acid, p-methyl benzenesulfonic acid etc.Because the acid catalyzed reaction of liquid belongs to homogeneous reaction, catalytic activity is high, but liquid acid catalyst exists etching apparatus, difficulty and product separation, is difficult to the difficult problems such as recycling.
Because solid acid has easily and the advantage such as product separation, recyclable recycling, be subject to the extensive concern of academia and industrial quarters in recent years.The solid acid catalyst reported at present comprises the heteropllyacids such as phosphomolybdic acid, silico-tungstic acid, the cationic ion-exchange resin classes such as Amberlyst-15, zeolite molecular sieve class etc., and wherein after the reaction of heteropllyacids compound, easily generating portion is dissolved, not easily recycling; Cationic ion-exchange resin class easily occurs swelling and broken in catalyse organic reaction process; Zeolite molecular sieve then there is acid strength and the drawbacks such as limited are measured in acid.
For above-mentioned existing solid acid catalyst synthesis Problems existing, the invention discloses a kind of is raw material with metal chloride, by hydrolysis, neutralization, ageing, washing, oven dry, obtain the method mixed with ammonium salt after pressed powder fully grinds, novel solid acid catalyst is prepared in roasting.
Summary of the invention
The object of the invention is to overcome existing solid acid catalyst easy generating portion in catalytic reaction dissolve, swelling and broken, not easily recycling, acid strength and the limited problem of acid amount.
For this reason, the invention provides a kind of preparation method of solid acid catalyst, comprise the steps:
Step 1) hydrolysis: by the ratio mixed dissolution of metal chloride and water 1:5 ~ 1:100 in mass ratio;
Step 2) neutralization: adopt concentration be 5% ~ 30% alkali lye by the metal chloride solutions after dissolving, to be adjusted to pH be 8 ~ 10;
Step 3) ageing, washing: by the liquid after still aging 10 ~ 30 hours after neutralization, adopt deionized water washing 3 ~ 10 times;
Step 4) to dry: the solid after washing is placed in baking oven and dries, bake out temperature is 80 ~ 120
oc, drying time is 10 ~ 30 hours;
Step 5) fully being pulverized by the solid after drying lastly mixes with ammonium salt, and ammonium salt quality is 5% ~ 50% of pressed powder quality;
Step 6) powder mixed in step 5) is placed in Muffle furnace roasting, obtain solid acid catalyst, wherein, sintering temperature is 300 ~ 600
oc, roasting time is 3 ~ 15 hours.
Above-mentioned metal chloride is two or more in butter of tin, titanium tetrachloride, zirconium chloride, zinc chloride, iron chloride, aluminium chloride.
In the mixture of two or more metal chloride above-mentioned, metal molar percentage is respectively tin 1 ~ 20%, titanium 20 ~ 80%, zirconium 20 ~ 80%, zinc 0 ~ 15%, iron 0 ~ 20%, aluminium 0 ~ 15%.
Above-mentioned alkali lye is the one in NaOH, potassium hydroxide, ammoniacal liquor.
Above-mentioned concentration of lye is 2 ~ 20%.
Above-mentioned ammonium salt is one or more in ammonium chloride, ammonium sulfate, ammonium hydrogen sulfate, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate (ADP), ammonium nitrate.
Above-mentioned steps 5) in ammonium salt quality to account for pressed powder optimal quality be 10% ~ 25%.
Beneficial effect of the present invention:
(1) this solid acid catalyst that obtains of the present invention is compared with the solid acid catalyst of existing synthesis, and cheaper starting materials is easy to get, simple synthetic method is easy.
(2) solid acid catalyst for preparing of the preparation method of this solid acid catalyst provided by the invention acid strong, to recycle performance good, have broad application prospects.
Below with reference to accompanying drawing, the present invention is described in further details.
Accompanying drawing explanation
Fig. 1 is the infrared figure of pyridine of the solid acid catalyst that embodiment 1 is synthesized.
Fig. 2 is the infrared figure of pyridine of the solid acid catalyst of the 2-in-1 one-tenth of embodiment.
Fig. 3 is the NH of the solid acid catalyst that embodiment 1 is synthesized
3-TPD schemes.
Fig. 4 is the NH of the solid acid catalyst of the 2-in-1 one-tenth of embodiment
3-TPD schemes.
Fig. 5 is the TG-DTA figure of the solid acid catalyst of the 2-in-1 one-tenth of embodiment.
Detailed description of the invention
Embodiment 1:
Dissolve to overcome existing solid acid catalyst easy generating portion in catalytic reaction, swelling and broken, not easily recycling, limited problem is measured in acid strength and calculation, present embodiments provides a kind of preparation method of solid acid catalyst, comprises the steps:
Step 1) hydrolysis: take 7.012 g SnCl
45H
2o, 13.280 g TiCl
4, 2.414 g AlCl
36H
2o(metal molar percentage is 20%:70%:10%), be dissolved in 500 mL water, fully stir and make it all dissolve.
Step 2) neutralization: add in above-mentioned solution concentration be 10% sodium hydroxide solution be adjusted to pH=10.
Step 3) ageing, washing: by the solution left standstill ageing after 15 hours after neutralization, adopt deionized water to wash 3 times.
Step 4) dry: the solid after above-mentioned washing is placed in baking oven 100
oCdry 15 hours.
Step 5) pressed powder after drying fully is ground, crosses 200 mesh sieves, take a certain amount of ammonium hydrogen sulfate (quality is 10% of pressed powder), the powder after it being sieved with ground solid fully mixes.
Step 6) mixed pressed powder is placed in Muffle furnace, 500
oc roasting 10 h, obtains solid acid catalyst.
Infrared and the NH by pyridine
3-TPD characterizes the solid acid catalyst that the present embodiment obtains, and as shown in figures 1 and 3, shows that the solid acid catalyst synthesized is simultaneously containing Lewis acid position and Br nsted acid position, and contains a large amount of Br nsted strong acidic sites and super acids position.
Embodiment 2:
Take 7.012 g SnCl
45H
2o, 15.177 g TiCl
4, 1.363 g ZnCl
2(metal molar percentage is 10%:80%:10%), is dissolved in 450 mL water, abundant stirring and dissolving, add in solution concentration be 10% ammoniacal liquor be adjusted to pH=9; By the solution left standstill ageing after neutralization after 20 hours, adopt deionized water to wash 5 times, the solid after washing is placed in baking oven 90
oCdry 20 hours; Pressed powder after oven dry fully grinds, cross 100 mesh sieves, and take a certain amount of ammonium sulfate (quality is 20% of pressed powder), the powder after it being sieved with ground solid fully mixes; Mixed pressed powder is placed in Muffle furnace, 450
oc roasting 15 h, obtains solid acid catalyst.
Infrared and the NH by pyridine
3-TPD characterizes the solid acid catalyst that the present embodiment obtains, and result as shown in Figure 2 and Figure 4, shows that the solid acid catalyst synthesized is simultaneously containing Lewis acid position and Br nsted acid position, and contains a large amount of Br nsted strong acidic sites and super acids position.As shown in Figure 5, analyzed by TG-DTA, show that the solid acid catalyst synthesized has excellent heat endurance.
Embodiment 3:
Take 3.506 g SnCl
45H
2o, 18.656 g ZrCl
4, 1.363 g ZnCl
2, 1.207 g AlCl
36H
2o(metal molar percentage is 5%:80%:10%:5%), be dissolved in 750 mL water, abundant stirring and dissolving, add in solution concentration be 5% potassium hydroxide be adjusted to pH=8; By the solution left standstill ageing after neutralization after 10 hours, deionized water is adopted to wash 3 times; Solid after washing is placed in baking oven 80
oCdry 10 hours; Pressed powder after oven dry fully grinds, cross 100 mesh sieves, and take the mixture of a certain amount of ammonium sulfate and ammonium chloride, its gross mass is 5% of pressed powder, and the powder after it being sieved with ground solid fully mixes; Mixed pressed powder is placed in Muffle furnace, 300
oc roasting 3 h, obtains solid acid catalyst.
By characterizing, show that the solid acid catalyst that the present embodiment synthesizes contains Lewis acid position and Br nsted acid position simultaneously, and containing Br nsted strong acidic site and super acids position, and there is excellent heat endurance.
Embodiment 4:
Take 5.25 g SnCl
45H
2o, 18.656 g ZrCl
4, 1.352 g FeCl
36H
2o(metal molar percentage is 15%:80%:5%), be dissolved in 1000 mL water, abundant stirring and dissolving, add in solution concentration be 30% NaOH be adjusted to pH=10; By the solution left standstill ageing after neutralization after 30 hours, deionized water is adopted to wash 10 times; Solid after washing is placed in baking oven 120
oCdry 30 hours; Pressed powder after oven dry fully grinds, cross 100 mesh sieves, and take a certain amount of ammonium sulfate and ammonium hydrogen sulfate mixture (quality is 20% of pressed powder), the powder after it being sieved with ground solid fully mixes; Mixed pressed powder is placed in Muffle furnace, 600
oc roasting 15 h, obtains solid acid catalyst.
By characterizing, show that the solid acid catalyst synthesized is simultaneously containing Lewis acid position and Br nsted acid position, and containing Br nsted strong acidic site and super acids position, and there is excellent heat endurance.
Ammonium salt in above-described embodiment can also be one or more in ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate (ADP), ammonium nitrate.
In sum, the preparation method of this solid acid catalyst provided by the invention take metal chloride as raw material, by hydrolysis, neutralization, ageing, washing, oven dry, obtain the method mixed with ammonium salt after pressed powder fully grinds, novel solid acid catalyst is prepared in roasting, compared with the solid acid catalyst of existing synthesis, cheaper starting materials of the present invention is easy to get, simple synthetic method is easy, characterization result shows, the solid acid catalyst of synthesis is acid strong, it is good to recycle performance, has broad application prospects.
More than exemplifying is only illustrate of the present invention, does not form the restriction to protection scope of the present invention, everyly all belongs within protection scope of the present invention with the same or analogous design of the present invention.
Claims (7)
1. a preparation method for solid acid catalyst, is characterized in that: comprise the steps:
Step 1) hydrolysis: by the ratio mixed dissolution of metal chloride and water 1:5 ~ 1:100 in mass ratio;
Step 2) neutralization: adopt concentration be 5% ~ 30% alkali lye by the metal chloride solutions after dissolving, to be adjusted to pH be 8 ~ 10;
Step 3) ageing, washing: by the liquid after still aging 10 ~ 30 hours after neutralization, adopt deionized water washing 3 ~ 10 times;
Step 4) to dry: the solid after washing is placed in baking oven and dries, bake out temperature is 80 ~ 120
oc, drying time is 10 ~ 30 hours;
Step 5) fully being pulverized by the solid after drying lastly mixes with ammonium salt, and ammonium salt quality is 5% ~ 50% of pressed powder quality;
Step 6) powder mixed in step 5) is placed in Muffle furnace roasting, obtain solid acid catalyst, wherein, sintering temperature is 300 ~ 600
oc, roasting time is 3 ~ 15 hours.
2. the preparation method of solid acid catalyst as claimed in claim 1, is characterized in that: described metal chloride is two or more in butter of tin, titanium tetrachloride, zirconium chloride, zinc chloride, iron chloride, aluminium chloride.
3. the preparation method of solid acid catalyst as claimed in claim 2, is characterized in that: in the mixture of two or more metal chloride described, metal molar percentage is respectively tin 1 ~ 20%, titanium 20 ~ 80%, zirconium 20 ~ 80%, zinc 0 ~ 15%, iron 0 ~ 20%, aluminium 0 ~ 15%.
4. the preparation method of solid acid catalyst as claimed in claim 1, is characterized in that: described alkali lye is the one in NaOH, potassium hydroxide, ammoniacal liquor.
5. the preparation method of solid acid catalyst as claimed in claim 4, is characterized in that: described concentration of lye is 2 ~ 20%.
6. the preparation method of solid acid catalyst as claimed in claim 1, is characterized in that: described ammonium salt is one or more in ammonium chloride, ammonium sulfate, ammonium hydrogen sulfate, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate (ADP), ammonium nitrate.
7. the preparation method of solid acid catalyst as claimed in claim 1, is characterized in that: described step 5) in ammonium salt quality to account for pressed powder optimal quality be 10% ~ 25%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106513024A (en) * | 2016-10-20 | 2017-03-22 | 陕西延长石油（集团）有限责任公司炼化公司 | Solid acid catalyst, and preparation method and application thereof |
| CN106554277A (en) * | 2016-10-20 | 2017-04-05 | 陕西延长石油（集团）有限责任公司炼化公司 | A kind of solid acid catalysis synthesize the method for Isosorbide-5-Nitrae butylene glycol aerylate |
| CN112973663A (en) * | 2021-03-12 | 2021-06-18 | 盐城工学院 | Solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearic acid and preparation method thereof |
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| 牛梅菊等: "固体酸SO42-/TiO2-Al2O3-SnO2催化合成氯乙酸四甘醇双酯", 《精细化工》 * |
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| CN106513024A (en) * | 2016-10-20 | 2017-03-22 | 陕西延长石油（集团）有限责任公司炼化公司 | Solid acid catalyst, and preparation method and application thereof |
| CN106554277A (en) * | 2016-10-20 | 2017-04-05 | 陕西延长石油（集团）有限责任公司炼化公司 | A kind of solid acid catalysis synthesize the method for Isosorbide-5-Nitrae butylene glycol aerylate |
| CN112973663A (en) * | 2021-03-12 | 2021-06-18 | 盐城工学院 | Solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearic acid and preparation method thereof |
| CN112973663B (en) * | 2021-03-12 | 2023-03-10 | 盐城工学院 | Solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearate and preparation method thereof |
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