CN104815689B - A kind of HPPO Catalyst Productions technological process - Google Patents
A kind of HPPO Catalyst Productions technological process Download PDFInfo
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- CN104815689B CN104815689B CN201510115277.3A CN201510115277A CN104815689B CN 104815689 B CN104815689 B CN 104815689B CN 201510115277 A CN201510115277 A CN 201510115277A CN 104815689 B CN104815689 B CN 104815689B
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 230000008569 process Effects 0.000 title claims abstract description 33
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- HWOWEGAQDKKHDR-UHFFFAOYSA-N 4-hydroxy-6-(pyridin-3-yl)-2H-pyran-2-one Chemical compound O1C(=O)C=C(O)C=C1C1=CC=CN=C1 HWOWEGAQDKKHDR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000002425 crystallisation Methods 0.000 claims abstract description 27
- 230000008025 crystallization Effects 0.000 claims abstract description 27
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 8
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims abstract description 7
- 230000004913 activation Effects 0.000 claims abstract description 6
- 239000004033 plastic Substances 0.000 claims abstract description 6
- 239000002808 molecular sieve Substances 0.000 claims description 22
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 206010013786 Dry skin Diseases 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 230000003020 moisturizing effect Effects 0.000 claims description 3
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- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- QQONPFPTGQHPMA-UHFFFAOYSA-N Propene Chemical compound CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 abstract description 8
- 238000001994 activation Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 abstract description 4
- 238000011109 contamination Methods 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 4
- 238000006735 epoxidation reaction Methods 0.000 abstract description 4
- 239000007800 oxidant agent Substances 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 239000001294 propane Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- -1 4-propyl bromide Chemical compound 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- ZXVOCOLRQJZVBW-UHFFFAOYSA-N azane;ethanol Chemical compound N.CCO ZXVOCOLRQJZVBW-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 239000003292 glue Substances 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000011964 heteropoly acid Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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Abstract
The present invention relates to a kind of HPPO Catalyst Productions technological process, its raw material includes tetraethyl orthosilicate, butyl titanate, TPAOH (TPAOH), 4-propyl bromide (TPABr), isopropanol etc., equipment includes crystallization device, storage tank, filter plant, heat exchanger, pump, air compressor machine etc., and its technological process of production includes the processes such as plastic, ageing, crystallization, alkali process, acid activation, separation, drying, roasting.Using the HPPO catalyst that the technological process of production is prepared in catalysis preparing epoxypropane by epoxidation of propene reaction, free of contamination low concentration hydrogen peroxide can be used as oxidant, the problem of avoiding complicated traditional handicraft process and pollution environment, with traditional system unrivaled energy-conservation, economy and advantages of environment protection, and there is good reaction selectivity, there is good prospects for commercial application.
Description
Technical field
The present invention relates to catalyst preparation production field, especially a kind of HPPO Catalyst Productions technological process.
Background technology
HPPO methods are the new technologies of hydrogen peroxide catalyzed epoxidation propylene production expoxy propane, and ring is only produced in production process
Ethylene Oxide and water.Compared with traditional Synthesis of Propylene Oxide, HPPO technical process is simple, and process unit floor space is small,
Required auxiliary facility is also less, and investment and cost can reduce 25%, and discharge of wastewater can reduce 70%-80%, and energy consumption can be reduced
35%, while product yield is high, no coupling product is pollution-free, belongs to cleaning procedure.
During HPPO methods produce expoxy propane, the selection of catalyst is even more important, domestic that the method is catalyzed in recent years
The selection of agent has carried out developmental research, and good effect is achieved with tungsten-containing catalyst and phosphoric acid heteropolyacid salt catalyst.TS-1
HTS is with excellent by one kind formed in framework of molecular sieve of the transition metal titanium introducing with MFI structure
Clean catalytic oxidization performance novel titanosilicate, it is identical with the skeleton structure of ZSM-5 molecular sieve.TS-1 molecular sieves are not only
Catalysed oxidn with titanium, but also the shape-selective effect with MFI molecular sieves and excellent stability.
TS-1 molecular sieves can use free of contamination low concentration peroxide in catalysis preparing epoxypropane by epoxidation of propene reaction
Change hydrogen as oxidant, the problem of avoiding traditional handicraft process complexity and pollute environment, have traditional system unrivaled
Energy-conservation, economy and advantages of environment protection, and there is good reaction selectivity, there is good prospects for commercial application.
The content of the invention
The main object of the present invention is to provide a kind of HPPO Catalyst Productions technological process, including plastic, ageing, crystallization,
The processes such as alkali process, acid activation, separation, drying, roasting.Using the HPPO catalyst that the technique is prepared in catalysis propylene ring
Oxidation is prepared in expoxy propane reaction, and free of contamination low concentration hydrogen peroxide can be used to avoid traditional handicraft as oxidant
The problem of process is complicated and pollutes environment, there is traditional system unrivaled energy-conservation, economy and advantages of environment protection, and have
There is good reaction selectivity, there is good prospects for commercial application.
According to HPPO Catalyst Production technological processes, its raw material includes tetraethyl orthosilicate, butyl titanate, tetrapropyl hydrogen-oxygen
Change ammonium, 4-propyl bromide, isopropanol etc.；Equipment includes crystallization device, storage tank, filter plant, heat exchanger, pump, air compressor machine
Deng.Its technological process of production includes the processes such as plastic, ageing, crystallization, alkali process, acid activation, separation, drying, roasting.
Technique is sketched：
(1) plastic：By distilled water, tetraethyl orthosilicate and TPABr with mol ratio (150~200): (5~10): 1 is added to
In crystallization device, it is 9~11 to adjust pH with ethanol ammonium, 0.5~2h is stirred at room temperature, by H2O2Solution, butyl titanate, isopropyl
Alcohol is with mol ratio (1~6): 1: after (20~30) are well mixed, be slowly added into above-mentioned crystallization device, wherein butyl titanate
Be 1 with the mol ratio of tetraethyl orthosilicate: (30~70), 0.5~2h be stirred at room temperature, be warming up to 60~90 DEG C and remove alcohol, during it is suitable
Work as moisturizing, altogether except 2~5h of alcohol, obtain colloidal sol.
(2) it is aged：A small amount of TS-1 molecular sieve seeds are added into above-mentioned colloidal sol, at room temperature 2~24h of sealing ageing.
(3) crystallization：120~200 DEG C of 12~150h of crystallization, filtered, washing, 110~150 DEG C of dryings are warming up to after ageing
3~10h is calcined after 350~800 DEG C, obtains TS-1 molecular screen primary powders.
(4) alkali process：By water, TPAOH and TS-1 molecular screen primary powders by weight (5~50): (0.5~5): 1 adds successively
Enter into crystallization device, 0.5~5h is stirred at room temperature, 120~200 DEG C of 12~150h of crystallization, filtered, water are warming up under sealing
Wash, obtain the TS-1 molecular sieves after alkali process after 110~150 DEG C of dryings.
(5) acid activation：By H2SO4Solution (0.25M), H2O2TS-1 molecular sieves after solution, alkali process are with weight ratio (10
~30): (0.5~5): 1 is added sequentially in the tank diameter with heating, it is warming up to processing 1~6h, filtered, washing, 110~
150 DEG C of dryings are calcined 3~10h after 350~800 DEG C, obtain HPPO catalyst.
Compared with prior art H is added during plastic2O2Complex compound is formed with titanium, prevents the hydrolytic precipitation of butyl titanate,
Butyl titanate is protected, suppresses the hydrolysis of butyl titanate, adds the hydrolysis that isopropanol suppresses butyl titanate so that the water of butyl titanate
Solution speed is suitable with the hydrolysis rate of tetraethyl orthosilicate, and the formation to TS-1 molecular sieves has great role.The present invention is in alkali process
After secondary crystallization again introduce acid treatment activation the step of can effective selectivity removing molecular sieve in extra-framework titanium, it is modified to urge
Agent activity is improved significantly, and hydrogen peroxide can aid in removing the extra-framework titanium in molecular sieve.
It is anti-in catalysis preparing epoxypropane by epoxidation of propene using the HPPO catalyst that the technological process of production is prepared
Ying Zhong, free of contamination low concentration hydrogen peroxide can be used to avoid traditional handicraft process complexity and pollution environment as oxidant
The problem of, there is traditional system unrivaled energy-conservation, economy and advantages of environment protection, and there is good selecting response
Property, there is good prospects for commercial application.
Embodiment
Embodiment 1
(1) 205kg distilled water, 129kg tetraethyl orthosilicates, 19.26kg ethanol ammonium and 17.20kg TPABr are sequentially added
30min is stirred at room temperature into crystallization device, adds 8.26kg H2O2, 5min is stirred, 4.6kg butyl titanates are dissolved in 18.2kg
After isopropanol is well mixed, it is slowly added into above-mentioned crystallization device (about 30min is added), 1h is stirred at room temperature, is warming up to 80
DEG C alcohol is removed, per 30min moisturizings to liquid level before alcohol is removed, altogether except alcohol 3h, obtain colloidal sol.
(2) 1.65kg TS-1 molecular sieve seeds are added into above-mentioned colloidal sol, at room temperature sealing ageing 24h.
(3) 175 DEG C of crystallization 72h are warming up to after being aged, are obtained after filtered, washing and 120 DEG C of dryings, 550 DEG C of roasting 6h
TS-1 molecular screen primary powders.
(4) by part by weight be 11.5: 1.5: 1 water, TPAOH and TS-1 molecular screen primary powders be added sequentially to stirring crystalline substance
Change in reactor, 2h is stirred at room temperature, 175 DEG C of crystallization 48h are warming up under sealing, alkali is obtained after filtered, washing and 120 DEG C of dryings
TS-1 molecular sieves after processing.
(5) it is 15 (L): 1.5 (kg): 1 (kg) H by ratio2SO4Solution (0.25M), H2O2Solution (27.5wt%), alkali
TS-1 molecular sieves after processing are added sequentially to stir in the tank diameter with heating, are warming up to 85 DEG C of processing 2.5h, filtered, water
Wash, 550 DEG C of roasting 6h after 120 DEG C of dryings, obtain HPPO catalyst.
Comparative example 1
Using Ludox, titanium sulfate, TPAOH is template, adds ammoniacal liquor regulation basicity, and deionized water presses 1
: 0.013-0.035: 0.025-0.2: 25-45: 15-35 ratio, wherein Si/TPA+=0.08 and different orders of addition mixing system
Glue, with ammoniacal liquor (NH3) regulation glue basicity, crystal seed is added, and ceaselessly stir, after stirring 1-5 hours, made coagulant liquid is turned
Enter in the special polytetrafluoroethylene (PTFE) autoclave of microwave (30ml/100ml), adjust microwave power 400W-1600W, crystallization temperature
For 160-180 DEG C, crystallization 2-30h, cooling, filtering are then taken out, is repeatedly neutral to filtrate with distillation water washing, then passes through again
Dry (＞ 12 hours), 550 DEG C of high-temperature roasting 5-10 hours, obtain titanium-silicon molecular sieve TS-1 original powder.By the TS-1 of above-mentioned gained
Former powder mixes with ammonia spirit, 130-190 DEG C of regulation PH 8-13 keeping temperatures, and crystallization 24-72 is small again under autogenous hydrothermal pressure
When, after filtration, washing and drying, at 500-600 DEG C be calcined 5-6 hours obtain titanium-silicon molecular sieve catalyst sample.
Comparative example 2
In the first step, the TS-1 molecular screen primary powders that are not calcined: weight ratio=1: 50 of acid compound solution, acid chemical combination
The concentration of thing solution is 2.0mol/l, and acid compound is nitric acid；
In second step, reactant mixture made from the first step reacts 20 hours at 120 DEG C obtains titanium molecular sieve catalysis
Agent sample.
Comparative example 3
400 grams of propylene, the HTS that 12 grams of SiO2/TiO2 mol ratios are 50 are added in 2 liters of stainless steel reactors
TS-1 catalyst, reaction pressure 2.8MPa, 40 DEG C are heated to, then add 60 gram of 30 weight %H2O2, under agitation, reaction
Obtain titanium-silicon molecular sieve catalyst sample within 20 hours.
Catalyst is as follows for HPPO test result contrast：
XH2O2：Hydrogen peroxide conversion ratio；
SPO：Expoxy propane selectivity；
YPO：Expoxy propane yield；
UH2O2：Hydrogen peroxide effective rate of utilization.
Claims (3)
1. a kind of HPPO Catalyst Productions technological process, it is characterised in that comprise the following steps：
(1) plastic：Distilled water, tetraethyl orthosilicate and TPABr are added in crystallization device, it is 9~11 to adjust pH with monoethanolamine,
0.5~2h is stirred at room temperature, by H2O2Above-mentioned crystallization is slowly added into after solution, butyl titanate, isopropanol are well mixed
In device, 0.5~2h is stirred at room temperature, is warming up to 60~90 DEG C and removes alcohol, during appropriate moisturizing, altogether except 2~5h of alcohol, obtain colloidal sol；
(2) it is aged：A small amount of TS-1 molecular sieve seeds are added into above-mentioned colloidal sol, at room temperature 2~24h of sealing ageing, TS-1 molecules
The mol ratio for sieving crystal seed and tetraethyl orthosilicate is 1：(150~200)；
(3) crystallization：Be warming up to 120~200 DEG C of crystallization 12~150h after ageing, filtered, washing, 110~150 DEG C of dryings after
350~800 DEG C of 3~10h of roasting, obtain TS-1 molecular screen primary powders,
(4) alkali process：Water, TPAOH and TS-1 molecular screen primary powders are added sequentially in crystallization device, it is stirred at room temperature 0.5~
5h, 120~200 DEG C of 12~150h of crystallization are warming up under sealing, alkali process is obtained after filtered, washing, 110~150 DEG C of dryings
TS-1 molecular sieves afterwards,
(5) acid activation：By 0.25M H2SO4Solution, H2O2TS-1 molecular sieves after solution, alkali process are added sequentially to heating
In tank diameter, 1~6h of heating treatment, filtered, washing, 110~150 DEG C of dryings are calcined 3~10h after 350~800 DEG C, obtained
To HPPO catalyst；Distilled water, tetraethyl orthosilicate and TPABr are with mol ratio (150~200) in step (1): (5~10): 1 adds
Enter into crystallization device, H2O2Solution, butyl titanate, isopropanol are with mol ratio (1~6): 1: (20~30) are well mixed, its
The mol ratio of middle butyl titanate and tetraethyl orthosilicate is 1: (30~70).
2. HPPO Catalyst Productions technological process according to claim 1, it is characterised in that step (4) reclaimed water, TPAOH
And TS-1 molecular screen primary powders are by weight (5~50): (0.5~5): 1 is added sequentially in crystallization device.
3. HPPO Catalyst Productions technological process according to claim 1, it is characterised in that 0.25M in step (5)
H2SO4Solution, H2O2TS-1 molecular sieves after solution, alkali process are with weight ratio (10~30): (0.5~5): 1 is added sequentially to band
In the tank diameter of heating.
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|---|---|---|---|---|
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