CN103406134A - Aluminum oxide carrier solid alkali catalyst and preparation method thereof - Google Patents
Aluminum oxide carrier solid alkali catalyst and preparation method thereof Download PDFInfo
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- CN103406134A CN103406134A CN2013102875821A CN201310287582A CN103406134A CN 103406134 A CN103406134 A CN 103406134A CN 2013102875821 A CN2013102875821 A CN 2013102875821A CN 201310287582 A CN201310287582 A CN 201310287582A CN 103406134 A CN103406134 A CN 103406134A
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Abstract
The invention provides an aluminum oxide carrier solid alkali catalyst composed of the following components in parts by weight: 15-25 parts of calcium chloride, 15-25 parts of magnesium chloride, 3-5 parts of nano strontium titanate, 30-50 parts of nano aluminum oxide, 10-20 parts of ammonium molybdate, 5-10 parts of potassium carbonate and 0.5-1.5 parts of magnesium silicide. The aluminum oxide carrier solid alkali catalyst provided by the invention can be used as an organic synthesis reaction catalyst to significantly improve the conversion rate of chemical reactions and improve the product yield.
Description
Technical field
The present invention relates to the solid base catalyst preparing technical field, relate in particular to a kind of preparation method of alumina carrier solid base catalyst.
Background technology
Solid base catalyst is a kind of novel catalyst, high activity, high selectivity, chemical reaction condition are gentle because having, reaction system is easily separated, etching apparatus not, environmental friendliness, the advantage such as can reuse and more and more be paid attention to, especially aspect synthetic at fine chemistry, Polymer Synthesizing, the chemosynthesis reaction of a lot of severe reaction conditions can be carried out, and make the synthesis process serialization, reduced energy resource consumption, reduced the pollution to environment, in recent years the research and development of solid base also come extensively.Yet because solid base is novel catalyst, start to walk more late, especially preparing aspect solid base, preparation technology requires very meticulous, the cost costliness, the at present actual kind that is applied to industrial solid base catalyst is also very limited.Therefore need the multiple solid base catalyst for the different chemical reaction of exploitation to satisfy the demand.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of alumina carrier solid base catalyst, the above-mentioned defect existed to overcome prior art.
The invention provides a kind of alumina carrier solid base catalyst, formed by the component of following weight portion:
Described nano-aluminium oxide, particle diameter are the 40-80 nanometer;
The particle diameter of described nano strontium titanate is the 60-80 nanometer.
The present invention also provides a kind of preparation method of alumina carrier solid base catalyst, comprises the steps:
A), be dissolved into after calcium chloride 15-25 part, magnesium chloride 15-25 part are mixed in 250 parts, water, be made into mixed liquor;
B), in reactor, nano-aluminium oxide 30-50 part, nano strontium titanate 3-5 part and 500 parts of mixing of water are obtained to still bed material, high speed dispersion;
C), by mass concentration 15-25% ammoniacal liquor 50-100 part, and steps A) in the preparation mixed liquor add simultaneously step B) the still bed material in, under room temperature the reaction 1-2 hour; Then be warming up to 80 ℃-90 ℃, continue reaction 2-3 hour;
D) be down to normal temperature, separate and remove foreign ion, drying after obtain sediment;
E) by D) sediment that obtains of step is at 550-610 ℃ of lower roasting 3-4 hour, obtains calcining matter;
F) will after described calcining matter taking-up, directly add in normal-temperature water instantaneous temperature reduction, then separation, dry, grind into powder;
G) by F) powder that obtains of step joins 1-5% ammonium molybdate solution 10-20 part, and will after 20 parts of dissolvings of potash 5-10 part water, add simultaneously, after mixing, at 100 ℃～120 ℃, being dried to moisture all evaporates, add again magnesium silicide 0.5-1.5 part, after 470-520 ℃ of lower roasting 1-2 hour, calcining matter is ground into powder, obtain the alumina carrier solid base catalyst.
The preparation method of described magnesium silicide can be referring to disclosed method preparation in " synthetic chemistry " (Chemical Industry Press, 2005 first impressions, the 60th page).
Alumina carrier solid base catalyst of the present invention is by the crystallization principle in chemical reaction process, by composite chemical, react and prepare crystal and recrystallization doping chemical reaction and make oxide surface doping and chemical coordination, impel between oxide and form mixed crystal, by temperature jump, change again the lattice of crystal, enlarge specific area, increase the alundum (Al2O3) load capacity, impel oxide surface to accept the combination position of proton, the intensity of raising alkali is other thulium catalyst of load also, can be used as the organic synthesis catalyst, significantly improve the conversion ratio of chemical reaction, improve the yield of product.
Alumina carrier solid base catalyst of the present invention especially be suitable for the preparation ultraviolet vapor isocyanuric acid three benzo triazoles in as catalyst, the chemical structural formula of described isocyanuric acid three benzo triazoles is as follows:
Concrete preparation technology is as follows:
(b). in reactor by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add again alumina carrier solid base catalyst and NaOH; with nitrogen protection, reacted 1～2 hour at 75 ℃～85 ℃; separate oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and water is accessory substance, and the sediment alumina carrier solid base catalyst in water is reclaimed.
Each composition weight umber is as follows: 15～30 parts of isocyanuric acids, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) 1～3 part of 100～300 parts of alumina carrier solid base catalyst of BTA; 5～10 parts, NaOH.
The specific embodiment
In embodiment, the consumption of component is weight portion.
Embodiment 1
One, alumina carrier solid base catalyst and preparation method pass through following steps:
(a). chemical constituent: 750 parts of deionized waters, 15 parts, calcium chloride, 25 parts, magnesium chloride, 3 parts of nano strontium titanates, 100 parts of 25% ammoniacal liquor, 30 parts of nano-aluminium oxides, 20 parts of 3% ammonium molybdate aqueous solutions, 5 parts, potash, 1.5 parts of magnesium silicides;
(b). by calcium chloride, magnesium chloride is dissolved in 250 parts of deionized waters after mixing, in reactor, add 500 parts of deionized waters, add nano-aluminium oxide and nano strontium titanate, opening high speed dispersor 1500 Zhuan ∕ divides, ammoniacal liquor is diluted to 250 parts with deionized water, all solution temperatures are controlled to 10 ℃, then by calcium chloride, magnesium chloride solution and ammoniacal liquor are added drop-wise in reactor simultaneously, dropwised in 10 minutes, high-speed stirred is 2 hours at 10 ℃ of temperature, then be warming up to 90 ℃, continued high-speed stirred 3 hours, stop stirring, be down to normal temperature, the suction filtration sediment, putting into 250 parts of deionized waters disperses again, foreign ion in the washing and precipitating thing, suction filtration sediment again, and at 100 ℃, be dried to moisture and all evaporate, (c). by the product of (b) process, 610 ℃ of lower roastings are after 3 hours, by in the disposable deionized water of pouring normal temperature into of calcining matter, instantaneous temperature reduction, the amount of deionized water is 10 times of calcining matter weight, suction filtration sediment again, and at 100 ℃, be dried to moisture content and all evaporate, and calcining matter is ground into powder,
(d). by the powder of (c) process, add again ammonium molybdate solution, and after being dissolved with the deionized water of 20 parts, potash adds simultaneously, fully mix, at 100 ℃, be dried to moisture and all evaporate, then add magnesium silicide, 470 ℃ of lower roastings after 2 hours, calcining matter is ground into powder, obtains the alumina carrier solid base catalyst.
Two, the preparation method of ultraviolet vapor isocyanuric acid three benzo triazoles, prepare by following steps;
(a). chemical constituent: 15 parts of isocyanuric acids, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) 1 part of 100 parts of alumina carrier solid base catalyst of BTA; 5 parts, NaOH
(b). in reactor by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add again alumina carrier solid base catalyst and NaOH; with nitrogen protection, reacted 1 hour at 85 ℃; separate oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and water is accessory substance, and the sediment alumina carrier solid base catalyst in water is reclaimed.
Embodiment 2
One, alumina carrier solid base catalyst and preparation method pass through following steps:
(a). chemical constituent: 750 parts of deionized waters, 25 parts, calcium chloride, magnesium chloride 15,5 parts of nano strontium titanates, 50 parts of 25% ammoniacal liquor, 50 parts of nano-aluminium oxides, 10 parts of 3% ammonium molybdate aqueous solutions, 10 parts, potash, 0.5 part of magnesium silicide;
(b). by calcium chloride, magnesium chloride is dissolved in 250 parts of deionized waters after mixing, in reactor, add 500 parts of deionized waters, add nano-aluminium oxide and nano strontium titanate, opening high speed dispersor 2000 Zhuan ∕ divides, ammoniacal liquor is diluted to 250 parts with deionized water, all solution temperatures are controlled to 20 ℃, then by calcium chloride, magnesium chloride solution and ammoniacal liquor are added drop-wise in reactor simultaneously, in 20 minutes, dropwise simultaneously, high-speed stirred is 1 hour at 20 ℃ of temperature, then be warming up to 80 ℃, continued high-speed stirred 3 hours, stop stirring, be down to normal temperature, the suction filtration sediment, putting into 250 parts of deionized waters disperses again, foreign ion in the washing and precipitating thing, suction filtration sediment again, and at 120 ℃, be dried to moisture and all evaporate,
(c). by the product of (b) process, 610 ℃ of lower roastings after 3 hours, by in the disposable deionized water of pouring normal temperature into of calcining matter, instantaneous temperature reduction, the amount of deionized water is 10 times of calcining matter weight, suction filtration sediment again, and at 120 ℃, be dried to moisture content and all evaporate, and calcining matter is ground into powder;
(d). by the powder of (c) process, add again ammonium molybdate solution, and after being dissolved with the deionized water of 20 parts, potash adds simultaneously, fully mix, at 120 ℃, be dried to moisture and all evaporate, then add magnesium silicide, 520 ℃ of lower roastings after 1 hour, calcining matter is ground into powder, obtains the alumina carrier solid base catalyst.
Two, the preparation method of ultraviolet vapor isocyanuric acid three benzo triazoles, prepare by following steps;
(a). chemical constituent: 30 parts of isocyanuric acids, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) 3 parts of 300 parts of alumina carrier solid base catalysts of BTA; 10 parts, NaOH;
(b). in reactor by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add again solid base catalyst and NaOH; with nitrogen protection, reacted 2 hours at 75 ℃; separate oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and water is accessory substance, and the sediment alumina carrier solid base catalyst in water is reclaimed.
Embodiment 3
One, alumina carrier solid base catalyst and preparation method pass through following steps:
(a). chemical constituent: 750 parts of deionized waters, 20 parts, calcium chloride, 20 parts, magnesium chloride, 4 parts of nano strontium titanates, 75 parts of 25% ammoniacal liquor, 40 parts of nano-aluminium oxides, 15 parts of 3% ammonium molybdate aqueous solutions, 7.5 parts, potash, 1 part of magnesium silicide;
(b). by calcium chloride, magnesium chloride is dissolved in 250 parts of deionized waters after mixing, in reactor, add 500 parts of deionized waters, add nano-aluminium oxide and nano strontium titanate, opening high speed dispersor 1750 ∕ divides, ammoniacal liquor is diluted to 250 parts with deionized water, all solution temperatures are controlled to 15 ℃, then by calcium chloride, magnesium chloride solution and ammoniacal liquor are added drop-wise in reactor simultaneously, dropwised in 15 minutes, high-speed stirred is 1.5 hours at 15 ℃ of temperature, then be warming up to 85 ℃, continued high-speed stirred 2.5 hours, stop stirring, be down to normal temperature, the suction filtration sediment, putting into 250 parts of deionized waters disperses again, foreign ion in the washing and precipitating thing, suction filtration sediment again, and at 110 ℃, be dried to moisture and all evaporate,
(c). by the product of (b) process, 580 ℃ of lower roastings after 3.5 hours, by in the disposable deionized water of pouring normal temperature into of calcining matter, instantaneous temperature reduction, the amount of deionized water is 10 times of calcining matter weight, suction filtration sediment again, and at 110 ℃, be dried to moisture content and all evaporate, calcining matter is ground into powder;
(d). by the powder of (c) process, add again ammonium molybdate solution, and after being dissolved with the deionized water of 20 parts, potash adds simultaneously, fully mix, at 110 ℃, be dried to moisture and all evaporate, then add magnesium silicide, 490 ℃ of lower roastings after 1.5 hours, calcining matter is ground into powder, obtains the alumina carrier solid base catalyst.
Two, the preparation method of ultraviolet vapor isocyanuric acid three benzo triazoles, prepare by following steps;
(a). chemical constituent: 22.5 parts of isocyanuric acids, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) 2 parts of 200 parts of alumina carrier solid base catalysts of BTA; 7.5 parts, NaOH;
(b). in reactor by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add again alumina carrier solid base catalyst and NaOH; with nitrogen protection, reacted 1.5 hours at 80 ℃; separate oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and water is accessory substance, and the sediment alumina carrier solid base catalyst in water is reclaimed.
Comparative Examples
The preparation method of ultraviolet ray vapor isocyanuric acid three benzo triazoles, prepare by following steps;
(a). chemical constituent: 22.5 parts of isocyanuric acids, 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) 200 parts of BTAs, 7.5 parts, NaOH;
(b). in reactor by isocyanuric acid and 2-(2 '-hydroxyl-3 ' chloromethyl-5 '-aminomethyl phenyl)) BTA fully mixes; add again NaOH; with nitrogen protection, reacted 3 hours at 95 ℃; separate oil phase; by the distilled water extraction secondary of oil phase with 10 parts; oil phase is product, and water is accessory substance.
Alumina carrier solid base catalyst Basicity Determination and application testing result (table one)
From the detection data of table one, can determine, alumina carrier solid base catalyst of the present invention, be applied to the synthetic of ultraviolet vapor isocyanuric acid three benzo triazoles, not only can reduce chemical reaction temperature, Reaction time shorten, and the product yield significantly improves, obtained good effect.
Claims (4)
1. an alumina carrier solid base catalyst, is characterized in that, is comprised of the component of following weight portion:
2. a kind of alumina carrier solid base catalyst according to claim 1, is characterized in that, described nano-aluminium oxide, particle diameter are the 40-80 nanometer, and the particle diameter of described nano strontium titanate is the 60-80 nanometer.
3. the preparation method of an alumina carrier solid base catalyst, is characterized in that, comprises the steps:
A), be dissolved into after calcium chloride 15-25 part, magnesium chloride 15-25 part are mixed in 250 parts, water, be made into mixed liquor;
B), in reactor, nano-aluminium oxide 30-50 part, nano strontium titanate 3-5 part and 500 parts of mixing of water are obtained to still bed material, high speed dispersion;
C), by mass concentration 15-25% ammoniacal liquor 50-100 part, and steps A) in the preparation mixed liquor add simultaneously step B) the still bed material in, under room temperature the reaction 1-2 hour; Then be warming up to 80 ℃-90 ℃, continue reaction 2-3 hour;
D) be down to normal temperature, separate and remove foreign ion, drying after obtain sediment;
E) by D) sediment that obtains of step is at 550-610 ℃ of lower roasting 3-4 hour, obtains calcining matter;
F) will after described calcining matter taking-up, directly add in normal-temperature water instantaneous temperature reduction, then separation, dry, grind into powder;
G) by F) powder that obtains of step joins 1-5% ammonium molybdate solution 10-20 part, and will after 20 parts of dissolvings of potash 5-10 part water, add simultaneously, after mixing, at 100 ℃～120 ℃, being dried to moisture all evaporates, add again magnesium silicide 0.5-1.5 part, after 470-520 ℃ of lower roasting 1-2 hour, calcining matter is ground into powder, obtain the alumina carrier solid base catalyst.
4. method according to claim 3, is characterized in that, nano-aluminium oxide, particle diameter are the 40-80 nanometer, and the particle diameter of described nano strontium titanate is the 60-80 nanometer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104014338A (en) * | 2014-06-12 | 2014-09-03 | 上海东升新材料有限公司 | Solid alkali carrier rare metal element catalyst and preparation method thereof |
| CN110496613A (en) * | 2019-09-11 | 2019-11-26 | 万华化学集团股份有限公司 | A kind of hydrogenation catalyst, preparation method and the method for preparing adjacent bis aminomethyl hexamethylene |
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| US20120304529A1 (en) * | 2009-09-01 | 2012-12-06 | Kior, Inc. | Temperature-Optimized Conversion of Lignocellulosic Biomass |
| 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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2013
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120304529A1 (en) * | 2009-09-01 | 2012-12-06 | Kior, Inc. | Temperature-Optimized Conversion of Lignocellulosic Biomass |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104014338A (en) * | 2014-06-12 | 2014-09-03 | 上海东升新材料有限公司 | Solid alkali carrier rare metal element catalyst and preparation method thereof |
| CN104014338B (en) * | 2014-06-12 | 2016-03-02 | 上海东升新材料有限公司 | Solid base carrier thallium catalyst and preparation method |
| CN110496613A (en) * | 2019-09-11 | 2019-11-26 | 万华化学集团股份有限公司 | A kind of hydrogenation catalyst, preparation method and the method for preparing adjacent bis aminomethyl hexamethylene |
| 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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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 |