CN103406134B - Preparation method of a kind of Aluminum oxide carrier solid alkali catalyst and products thereof - Google Patents
Preparation method of a kind of Aluminum oxide carrier solid alkali catalyst and products thereof Download PDFInfo
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- CN103406134B CN103406134B CN201310287582.1A CN201310287582A CN103406134B CN 103406134 B CN103406134 B CN 103406134B CN 201310287582 A CN201310287582 A CN 201310287582A CN 103406134 B CN103406134 B CN 103406134B
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Abstract
The preparation method that the invention provides a kind of Aluminum oxide carrier solid alkali catalyst and the product obtained according to the method, described preparation method utilizes the crystallization principle in chemical reaction process, by composite chemical reaction prepare crystal and recrystallization doping chemical reaction make oxide surface adulterate and chemical coordination, impel between oxide and form mixed crystal, the lattice of crystal is changed again by temperature jump, expand specific area, increase alundum (Al2O3) load capacity, oxide surface is impelled to accept the bound site of proton, improve intensity also other thulium catalyst of load of alkali, can be used as organic synthesis catalyst, significantly improve the conversion ratio of chemical reaction, improve the yield of product.
Description
Technical field
The present invention relates to solid base catalyst preparing technical field, particularly relate to a kind of preparation method of Aluminum oxide carrier solid alkali catalyst.
Background technology
Solid base catalyst is a kind of novel catalyst, because having, high activity, high selectivity, chemical reaction condition are gentle, reaction system is easily separated, not etching apparatus, environmental friendliness, the advantage such as can to reuse and more and more be paid attention to, especially in fine chemistry synthesis, Polymer Synthesizing, the chemosynthesis reaction of a lot of severe reaction conditions is carried out, and make synthesis process serialization, reduce energy resource consumption, decrease the pollution to environment, in recent years the research and development of solid base are also come extensively.But because of solid base be novel catalyst, start to walk more late, especially preparing in solid base, preparation technology requires very meticulous, cost intensive, and the actual kind being applied to industrial solid base catalyst is also very limited at present.Therefore need to develop the multiple solid base catalyst for different chemical reaction to satisfy the demand.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Aluminum oxide carrier solid alkali catalyst, to overcome the above-mentioned defect that prior art exists.
A first aspect of the present invention, provides a kind of preparation method of Aluminum oxide carrier solid alkali catalyst, comprises the steps:
A), by after calcium chloride 15-25 part, the mixing of magnesium chloride 15-25 part be dissolved in 250 parts, water, be made into mixed liquor;
B), in the reactor nano-aluminium oxide 30-50 part, nano strontium titanate 3-5 part and the mixing of 500 parts, water are obtained still bed material, high speed dispersion;
C), by mass concentration 15-25% ammoniacal liquor 50-100 part, and steps A) in the mixed liquor of preparation add step B simultaneously) still bed material in, react 1-2 hour under room temperature; Then be warming up to 80 DEG C-90 DEG C, continue reaction 2-3 hour;
D) be down to normal temperature, be separated and obtain sediment after removing foreign ion, drying;
E) by D) step obtain sediment roasting 3-4 hour at 550-610 DEG C, obtain calcining matter;
F) directly add in normal-temperature water after described calcining matter being taken out, instantaneous temperature reduction, then separation, dry, grind into powder;
G) by F) step obtain powder join 1-5% ammonium molybdate solution 10-20 part, and add after 20 parts, potash 5-10 part use water is dissolved simultaneously, after mixing, be dried to moisture at 100 DEG C ~ 120 DEG C all to evaporate, add magnesium silicide 0.5-1.5 part again, at 470-520 DEG C after roasting 1-2 hour, calcining matter is ground into powder, obtains Aluminum oxide carrier solid alkali catalyst.
The preparation method of described magnesium silicide can be prepared see method disclosed in " synthetic chemistry " (Chemical Industry Press, 2005 first printings, the 60th page).
Preferably, the particle diameter of described nano-aluminium oxide is 40-80 nanometer, and the particle diameter of described nano strontium titanate is 60-80 nanometer.
A second aspect of the present invention, provides a kind of Aluminum oxide carrier solid alkali catalyst, and described Aluminum oxide carrier solid alkali catalyst uses said method preparation and obtains.
Aluminum oxide carrier solid alkali catalyst of the present invention is by the crystallization principle in chemical reaction process, by composite chemical reaction prepare crystal and recrystallization doping chemical reaction make oxide surface adulterate and chemical coordination, impel between oxide and form mixed crystal, the lattice of crystal is changed again by temperature jump, expand specific area, increase alundum (Al2O3) load capacity, oxide surface is impelled to accept the bound site of proton, improve intensity also other thulium catalyst of load of alkali, can be used as organic synthesis catalyst, significantly improve the conversion ratio of chemical reaction, improve the yield of product.
Aluminum oxide carrier solid alkali catalyst of the present invention is especially suitable for preparing as catalyst in ultraviolet vapor isocyanuric acid three BTA, and the chemical structural formula of described isocyanuric acid three BTA is as follows:
Concrete preparation technology is as follows:
In a kettle. by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add Aluminum oxide carrier solid alkali catalyst and NaOH again; with nitrogen protection 75 DEG C ~ 85 DEG C reactions 1 ~ 2 hour; be separated oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and aqueous phase is accessory substance, the sediment Aluminum oxide carrier solid alkali catalyst in aqueous phase is reclaimed.
Wherein, each composition weight number is as follows: isocyanuric acid 15 ~ 30 parts, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA 100 ~ 300 parts, Aluminum oxide carrier solid alkali catalyst 1 ~ 3 part, 5 ~ 10 parts, NaOH.
Detailed description of the invention
In embodiment, the consumption of component is weight portion.
Embodiment 1
One, Aluminum oxide carrier solid alkali catalyst and preparation method pass through following steps:
(a). chemical constituent: deionized water 750 parts, 15 parts, calcium chloride, 25 parts, magnesium chloride, nano strontium titanate 3 parts, 25% ammoniacal liquor 100 parts, nano-aluminium oxide 30 parts, 3% ammonium molybdate aqueous solution 20 parts, 5 parts, potash, magnesium silicide 1.5 parts;
(b). by calcium chloride, be dissolved in 250 parts of deionized waters after magnesium chloride mixing, add 500 parts of deionized waters in a kettle., add nano-aluminium oxide and nano strontium titanate, open high speed dispersor 1500 revs/min, ammoniacal liquor deionized water is diluted to 250 parts, all solution temperatures are controlled at 10 DEG C, then by calcium chloride, magnesium chloride solution and ammoniacal liquor are added drop-wise in reactor simultaneously, within 10 minutes, dropwise, high-speed stirred 2 hours at 10 DEG C of temperature, then 90 DEG C are warming up to, continue high-speed stirred 3 hours, stop stirring, be down to normal temperature, suction filtration sediment, put into 250 parts of deionized water dispersions again, foreign ion in washing and precipitating thing, suction filtration sediment again, and be dried to moisture at 100 DEG C and all evaporate,
(c). by the product of (b) process, at 610 DEG C, roasting is after 3 hours, pour in the deionized water of normal temperature by disposable for calcining matter, instantaneous temperature reduction, the amount of deionized water is 10 times of calcining matter weight, suction filtration sediment again, and be dried to moisture content at 100 DEG C and all evaporate, and calcining matter is ground into powder;
(d). by the powder of (c) process, add ammonium molybdate solution again, and potash is added with after the deionized water dissolving of 20 parts simultaneously, fully mix, be dried to moisture at 100 DEG C all to evaporate, then add magnesium silicide, at 470 DEG C, roasting is after 2 hours, calcining matter is ground into powder, obtains Aluminum oxide carrier solid alkali catalyst.
Two, the preparation method of ultraviolet vapor isocyanuric acid three BTA, is prepared by following steps;
(a). chemical constituent: isocyanuric acid 15 parts, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA 100 parts of Aluminum oxide carrier solid alkali catalyst 1 part; 5 parts, NaOH
(b). in a kettle. by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add Aluminum oxide carrier solid alkali catalyst and NaOH again; with nitrogen protection 85 DEG C of reactions 1 hour; be separated oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and aqueous phase is accessory substance, the sediment Aluminum oxide carrier solid alkali catalyst in aqueous phase is reclaimed.
Embodiment 2
One, Aluminum oxide carrier solid alkali catalyst and preparation method pass through following steps:
(a). chemical constituent: deionized water 750 parts, 25 parts, calcium chloride, magnesium chloride 15, nano strontium titanate 5 parts, 25% ammoniacal liquor 50 parts, nano-aluminium oxide 50 parts, 3% ammonium molybdate aqueous solution 10 parts, 10 parts, potash, magnesium silicide 0.5 part;
(b). by calcium chloride, be dissolved in 250 parts of deionized waters after magnesium chloride mixing, add 500 parts of deionized waters in a kettle., add nano-aluminium oxide and nano strontium titanate, open high speed dispersor 2000 revs/min, ammoniacal liquor deionized water is diluted to 250 parts, all solution temperatures are controlled at 20 DEG C, then by calcium chloride, magnesium chloride solution and ammoniacal liquor are added drop-wise in reactor simultaneously, dropwised in 20 minutes simultaneously, high-speed stirred 1 hour at 20 DEG C of temperature, then 80 DEG C are warming up to, continue high-speed stirred 3 hours, stop stirring, be down to normal temperature, suction filtration sediment, put into 250 parts of deionized water dispersions again, foreign ion in washing and precipitating thing, suction filtration sediment again, and be dried to moisture at 120 DEG C and all evaporate,
(c). by the product of (b) process, at 610 DEG C, roasting is after 3 hours, pour in the deionized water of normal temperature by disposable for calcining matter, instantaneous temperature reduction, the amount of deionized water is 10 times of calcining matter weight, suction filtration sediment again, and be dried to moisture content at 120 DEG C and all evaporate, and calcining matter is ground into powder;
(d). by the powder of (c) process, add ammonium molybdate solution again, and potash is added with after the deionized water dissolving of 20 parts simultaneously, fully mix, be dried to moisture at 120 DEG C all to evaporate, then add magnesium silicide, at 520 DEG C, roasting is after 1 hour, calcining matter is ground into powder, obtains Aluminum oxide carrier solid alkali catalyst.
Two, the preparation method of ultraviolet vapor isocyanuric acid three BTA, is prepared by following steps;
(a). chemical constituent: isocyanuric acid 30 parts, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA 300 parts of Aluminum oxide carrier solid alkali catalyst 3 parts; 10 parts, NaOH;
(b). in a kettle. by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add solid base catalyst and NaOH again; with nitrogen protection 75 DEG C of reactions 2 hours; be separated oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and aqueous phase is accessory substance, the sediment Aluminum oxide carrier solid alkali catalyst in aqueous phase is reclaimed.
Embodiment 3
One, Aluminum oxide carrier solid alkali catalyst and preparation method pass through following steps:
(a). chemical constituent: deionized water 750 parts, 20 parts, calcium chloride, 20 parts, magnesium chloride, nano strontium titanate 4 parts, 25% ammoniacal liquor 75 parts, nano-aluminium oxide 40 parts, 3% ammonium molybdate aqueous solution 15 parts, 7.5 parts, potash, magnesium silicide 1 part;
(b). by calcium chloride, be dissolved in 250 parts of deionized waters after magnesium chloride mixing, add 500 parts of deionized waters in a kettle., add nano-aluminium oxide and nano strontium titanate, open high speed dispersor 1750/ point, ammoniacal liquor deionized water is diluted to 250 parts, all solution temperatures are controlled at 15 DEG C, then by calcium chloride, magnesium chloride solution and ammoniacal liquor are added drop-wise in reactor simultaneously, within 15 minutes, dropwise, high-speed stirred 1.5 hours at 15 DEG C of temperature, then 85 DEG C are warming up to, continue high-speed stirred 2.5 hours, stop stirring, be down to normal temperature, suction filtration sediment, put into 250 parts of deionized water dispersions again, foreign ion in washing and precipitating thing, suction filtration sediment again, and be dried to moisture at 110 DEG C and all evaporate,
(c). by the product of (b) process, at 580 DEG C, roasting is after 3.5 hours, pour in the deionized water of normal temperature by disposable for calcining matter, instantaneous temperature reduction, the amount of deionized water is 10 times of calcining matter weight, suction filtration sediment again, and be dried to moisture content at 110 DEG C and all evaporate, calcining matter is ground into powder;
(d). by the powder of (c) process, add ammonium molybdate solution again, and potash is added with after the deionized water dissolving of 20 parts simultaneously, fully mix, be dried to moisture at 110 DEG C all to evaporate, then add magnesium silicide, at 490 DEG C, roasting is after 1.5 hours, calcining matter is ground into powder, obtains Aluminum oxide carrier solid alkali catalyst.
Two, the preparation method of ultraviolet vapor isocyanuric acid three BTA, is prepared by following steps;
(a). chemical constituent: isocyanuric acid 22.5 parts, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA 200 parts of Aluminum oxide carrier solid alkali catalyst 2 parts; 7.5 parts, NaOH;
(b). in a kettle. by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add Aluminum oxide carrier solid alkali catalyst and NaOH again; with nitrogen protection 80 DEG C of reactions 1.5 hours; be separated oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and aqueous phase is accessory substance, the sediment Aluminum oxide carrier solid alkali catalyst in aqueous phase is reclaimed.
Comparative example
The preparation method of ultraviolet vapor isocyanuric acid three BTA, is prepared by following steps;
(a). chemical constituent: isocyanuric acid 22.5 parts, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA 200 parts, 7.5 parts, NaOH;
(b). in a kettle. by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add NaOH again; with nitrogen protection 95 DEG C of reactions 3 hours; be separated oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and aqueous phase is accessory substance.
Aluminum oxide carrier solid alkali catalyst Basicity Determination and application testing result (table one)
Can determine from the detection data of table one, Aluminum oxide carrier solid alkali catalyst of the present invention, is applied to the synthesis of ultraviolet vapor isocyanuric acid three BTA, not only can reduces chemical reaction temperature, Reaction time shorten, and product yield significantly improves, achieve excellent effect.
Claims (3)
1. a preparation method for Aluminum oxide carrier solid alkali catalyst, is characterized in that, comprises the steps:
A), by after calcium chloride 15-25 part, the mixing of magnesium chloride 15-25 part be dissolved in 250 parts, water, be made into mixed liquor;
B), in the reactor nano-aluminium oxide 30-50 part, nano strontium titanate 3-5 part and the mixing of 500 parts, water are obtained still bed material, high speed dispersion;
C), by mass concentration 15-25% ammoniacal liquor 50-100 part, and steps A) in the mixed liquor of preparation add step B simultaneously) still bed material in, react 1-2 hour under room temperature; Then be warming up to 80 DEG C-90 DEG C, continue reaction 2-3 hour;
D) be down to normal temperature, be separated and obtain sediment after removing foreign ion, drying;
E) by D) step obtain sediment roasting 3-4 hour at 550-610 DEG C, obtain calcining matter;
F) directly add in normal-temperature water after described calcining matter being taken out, instantaneous temperature reduction, then separation, dry, grind into powder;
G) by F) step obtain powder join 1-5% ammonium molybdate solution 10-20 part, and add after 20 parts, potash 5-10 part use water is dissolved simultaneously, after mixing, be dried to moisture at 100 DEG C ~ 120 DEG C all to evaporate, add magnesium silicide 0.5-1.5 part again, at 470-520 DEG C after roasting 1-2 hour, calcining matter is ground into powder, obtains Aluminum oxide carrier solid alkali catalyst.
2. the preparation method of Aluminum oxide carrier solid alkali catalyst according to claim 1, is characterized in that, the particle diameter of described nano-aluminium oxide is 40-80 nanometer, and the particle diameter of described nano strontium titanate is 60-80 nanometer.
3. an Aluminum oxide carrier solid alkali catalyst, is characterized in that, described Aluminum oxide carrier solid alkali catalyst uses preparation method as claimed in claim 1 or 2 and obtained.
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| CN110496613B (en) * | 2019-09-11 | 2022-04-22 | 万华化学集团股份有限公司 | Hydrogenation catalyst, preparation method thereof and method for preparing o-diaminomethylcyclohexane |
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| CN102847539A (en) * | 2012-09-29 | 2013-01-02 | 上海东升新材料有限公司 | Mixed crystal/solid alkali combined catalyst and preparation method thereof |
| CN103055860A (en) * | 2012-12-28 | 2013-04-24 | 上海东升新材料有限公司 | Composited crystal solid alkali supporter catalyst and preparation method |
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| CN103055860A (en) * | 2012-12-28 | 2013-04-24 | 上海东升新材料有限公司 | Composited crystal solid alkali supporter catalyst and preparation method |
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Denomination of invention: Preparation method and product of aluminum oxide carrier solid alkali catalyst Effective date of registration: 20191225 Granted publication date: 20160210 Pledgee: Bank of Hangzhou, Limited by Share Ltd, Shanghai branch Pledgor: Shanghai Dongsheng New Materials Co., Ltd. Registration number: Y2019310000035 |
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Date of cancellation: 20210813 Granted publication date: 20160210 Pledgee: Bank of Hangzhou Limited by Share Ltd. Shanghai branch Pledgor: SHANDONG DONGSHENG NEW MATERIAL Co.,Ltd. Registration number: Y2019310000035 |