CN101147872A - Method for preparing anhydrous formaldehyde industrial catalyst by methanol dehydrogenation - Google Patents
Method for preparing anhydrous formaldehyde industrial catalyst by methanol dehydrogenation Download PDFInfo
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- CN101147872A CN101147872A CNA2007101396684A CN200710139668A CN101147872A CN 101147872 A CN101147872 A CN 101147872A CN A2007101396684 A CNA2007101396684 A CN A2007101396684A CN 200710139668 A CN200710139668 A CN 200710139668A CN 101147872 A CN101147872 A CN 101147872A
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Abstract
The present invention discloses a preparation method of industrial catalyst for producing anhydrous formaldehyde by utilizing methyl alcohol dehydrogenation. Said preparation method includes the following steps: using (by wt%) 40%-60% of industrial sodium hydrogen carbonate as raw material, using 30%-20% of active carbon as adjuvant and using 30%-20% of bentonite as carrier, uniformly mixing them, then adding 5% of Na2SiO3 solution adhesive according to the solid-liquid ratio of 20:1, further uniformly mixing them, tabletting, drying, calcining, pulverizing and screening so as to obtain the invented product.
Description
Technical field
The present invention relates to a kind of Preparation of catalysts method, particularly is raw material with the industrial sodium bicarbonate, and active carbon is an auxiliary agent, and bentonite is a carrier, prepares a kind of preparation method who is used for the industrial catalyst of methanol dehydrogenation system anhydrous formaldehyde.
Technical background
In recent years, along with the increase of chemical products demands such as synthetic high-quality engineering plastics and methenamine, increasing to the demand of anhydrous formaldehyde.Except that independent use, anhydrous formaldehyde mainly is as the raw material of producing other chemical products, as producing the novel plastic polyformaldehyde, generating phenolic resins or Lauxite, production methenamine etc. with phenol or urea condensation.In addition, anhydrous formaldehyde also extensively obtains at aspects such as synthesized polymer material, newtype drug intermediate, senior spices, dyestuffs using.
Industrial production anhydrous formaldehyde adopts two-step method usually: at first with methanol oxidation (iron molybdenum method) or oxidative dehydrogenation (silver-colored method), generate water content up to the formalin more than 50%, and then concentrate formaldehyde with the technology of decompression distillation or solvent azeotropic, because the formalin vapour pressure is very low, and formaldehyde and water can also form azeotropic mixture, thereby in practical operation, the dehydration separating effect is not good, power consumption is huge, the production cost height.And, then can avoid the shortcoming of oxidizing process by methyl alcohol direct dehydrogenation system anhydrous formaldehyde, product formaldehyde is easy to separate with accessory substance hydrogen, can not only obtain high-quality hydrogen and avoid the separation problem of formalin.Producing anhydrous formaldehyde from methanol dehydrogenation is very popular in recent years research topic, mainly concentrate in the optimization of selection of catalysts and process conditions, but research still rests on laboratory stage, does not still have industrialized unit and occurs.
In the catalyst of having studied, it is a kind of to the effectively catalyst of methanol dehydrogenation system anhydrous formaldehyde that sodium carbonate is proved to be, but under study for action reagent sodium carbonate that adopts powdery more, there is the cost height, bed resistance is big, and easily the shortcoming that runs off is unsuitable for using in industrial production.
The inventor is a raw material with the industrial sodium bicarbonate, has studied the industrial sodium carbonate Preparation of catalysts process of methanol dehydrogenation system anhydrous formaldehyde, lays a good foundation for realizing the industrialization of producing the anhydrous formaldehyde process from methyl alcohol.
The invention provides a kind of preparation method who is used for the industrial catalyst of methanol dehydrogenation system anhydrous formaldehyde process.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with the industrial sodium bicarbonate, and active carbon is an auxiliary agent, and bentonite is a carrier, Na
2SiO
3Preparation method for the anhydrous formaldehyde industrial catalyst by methanol dehydrogenation of binding agent, to solve the inferior separating effect of dewatering in the existing method, consume energy big and the production cost height, and adopt pulverous reagent sodium carbonate to have the cost height, bed resistance is big, easily the problem that runs off.
The present invention adopts the industrial sodium bicarbonate raw material on the basis of present prior art, the preparation anhydrous formaldehyde industrial catalyst by methanol dehydrogenation, and its concrete process step is as follows:
With the industrial sodium bicarbonate is raw material, and active carbon is an auxiliary agent, and bentonite is a carrier, and its batching is formed (quality %) and is: industrial sodium bicarbonate 40%～60%, active carbon 30%～20%, bentonite 30%～20%.After these three kinds of components are evenly mixed, again with 5%Na as binding agent
2SiO
3Compressing tablet, drying, calcining, fragmentation, screening promptly got product after solution evenly mixed by 20: 1 solid-to-liquid ratio.Catalyst calcination temperature after the shaping is 673K, and calcination time is 1.5 hours.
The resulting catalyst of the present invention compares with the catalyst that existing laboratory research is adopted that to have a cost low, and the shaping of catalyst adjustable size is whole, and the characteristics that resistance is little can directly apply to the industrial production of methanol dehydrogenation system anhydrous formaldehyde.
The catalyst of above-mentioned preparation is used for methanol dehydrogenation system anhydrous formaldehyde, and its concrete process conditions are: reaction temperature: 973K; Reaction pressure: normal pressure; Air speed: 1.5ml/sg; Methanol feed concentration: 10%.With this understanding, methanol conversion is 63.14%, formaldehyde selectivity 71.53%, yield 45.16%.In the products obtained therefrom, contain formaldehyde 75%, contain methyl alcohol 25%.
Adopt catalyst provided by the invention in the process of methanol dehydrogenation system anhydrous formaldehyde, it is also advantageous in that has given full play to as the sodium carbonate of active component with as the common catalysis of the activated carbon of auxiliary agent, has improved the selectivity of formaldehyde.
The specific embodiment
Embodiment 1
With the industrial sodium bicarbonate is that raw material, active carbon are that auxiliary agent, bentonite are carrier, and batching is formed (quality %) and is: industrial sodium bicarbonate 50%, active carbon 20%, bentonite 30%.After these three kinds of components are evenly mixed, again with 5%Na as binding agent
2SiO
3Compressing tablet, drying, calcining, fragmentation, screening promptly got product after solution evenly mixed by 20: 1 solid-to-liquid ratio.Catalyst calcination temperature after the shaping is 673K, and calcination time is 1.5 hours.
Embodiment 2
According to the process of embodiment 1, its batching is formed (quality %): industrial sodium bicarbonate 50%, active carbon 30%, bentonite 20%.
Embodiment 3
According to the process of embodiment 1, its batching is formed (quality %): industrial sodium bicarbonate 60%, active carbon 20%, bentonite 20%.
Embodiment 4
According to the process of embodiment 1, its batching is formed (quality %): industrial sodium bicarbonate 40%, active carbon 30%, bentonite 30%.
Claims (5)
1. the preparation method of anhydrous formaldehyde industrial catalyst by methanol dehydrogenation is characterized in that it is to be raw material with the industrial sodium bicarbonate that catalyst is formed, and active carbon is an auxiliary agent, and bentonite is a carrier, Na
2SiO
3Be binding agent, its preparation process is to form quality % by the batching of catalyst to be: industrial sodium bicarbonate 40%～60%, active carbon 30%～20%, bentonite 30%～20%, and after its three kinds of components are mixed, add 5% Na again by 20: 1 solid-to-liquid ratio
2SiO
3The solution binding agent, compressing tablet, drying, calcining, fragmentation, screening promptly get product after mixing once more, catalyst calcination temperature after the moulding is 673K, and calcination time is 1.5 hours, and activity of such catalysts component sodium carbonate is to obtain by the sodium acid carbonate calcining and decomposing.
2. the preparation method of anhydrous formaldehyde industrial catalyst by methanol dehydrogenation as claimed in claim 1 is characterized in that the quality % of catalyst consists of: industrial sodium bicarbonate 50%, active carbon 20%, bentonite 30%.
3. the preparation method of anhydrous formaldehyde industrial catalyst by methanol dehydrogenation as claimed in claim 1 is characterized in that the quality % of catalyst consists of: industrial sodium bicarbonate 50%, active carbon 30%, bentonite 20%.
4. the preparation method of anhydrous formaldehyde industrial catalyst by methanol dehydrogenation as claimed in claim 1 is characterized in that the quality % of catalyst consists of: industrial sodium bicarbonate 60%, active carbon 20%, bentonite 20%.
5. the preparation method of anhydrous formaldehyde industrial catalyst by methanol dehydrogenation as claimed in claim 1 is characterized in that the quality % of catalyst consists of: industrial sodium bicarbonate 40%, active carbon 30%, bentonite 30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101396684A CN101147872A (en) | 2007-10-27 | 2007-10-27 | Method for preparing anhydrous formaldehyde industrial catalyst by methanol dehydrogenation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101396684A CN101147872A (en) | 2007-10-27 | 2007-10-27 | Method for preparing anhydrous formaldehyde industrial catalyst by methanol dehydrogenation |
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| CN101147872A true CN101147872A (en) | 2008-03-26 |
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| CNA2007101396684A Pending CN101147872A (en) | 2007-10-27 | 2007-10-27 | Method for preparing anhydrous formaldehyde industrial catalyst by methanol dehydrogenation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101961650A (en) * | 2010-09-10 | 2011-02-02 | 常州大学 | Zirconium base catalyst, preparation method and application in preparation of anhydrous formaldehyde |
| CN102872893A (en) * | 2012-09-03 | 2013-01-16 | 常州大学 | Catalyst used in process of preparing anhydrous formaldehyde by methanol dehydrogenation and preparation method and application process of catalyst |
| CN102941112A (en) * | 2012-11-21 | 2013-02-27 | 常州大学 | Novel catalyst for dehydrogenation preparation of formaldehyde by using methyl alcohol, preparation method and application of novel catalyst |
| CN104447242A (en) * | 2013-09-12 | 2015-03-25 | 中国科学院大连化学物理研究所 | Preparation method of anhydrous formaldehyde |
-
2007
- 2007-10-27 CN CNA2007101396684A patent/CN101147872A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101961650A (en) * | 2010-09-10 | 2011-02-02 | 常州大学 | Zirconium base catalyst, preparation method and application in preparation of anhydrous formaldehyde |
| CN101961650B (en) * | 2010-09-10 | 2012-08-29 | 常州大学 | Zirconium base catalyst, preparation method and application in preparation of anhydrous formaldehyde |
| CN102872893A (en) * | 2012-09-03 | 2013-01-16 | 常州大学 | Catalyst used in process of preparing anhydrous formaldehyde by methanol dehydrogenation and preparation method and application process of catalyst |
| CN102872893B (en) * | 2012-09-03 | 2014-06-18 | 常州大学 | Catalyst used in process of preparing anhydrous formaldehyde by methanol dehydrogenation and preparation method and application process of catalyst |
| CN102941112A (en) * | 2012-11-21 | 2013-02-27 | 常州大学 | Novel catalyst for dehydrogenation preparation of formaldehyde by using methyl alcohol, preparation method and application of novel catalyst |
| CN102941112B (en) * | 2012-11-21 | 2014-08-13 | 常州大学 | Novel catalyst for dehydrogenation preparation of formaldehyde by using methyl alcohol, preparation method and application of novel catalyst |
| CN104447242A (en) * | 2013-09-12 | 2015-03-25 | 中国科学院大连化学物理研究所 | Preparation method of anhydrous formaldehyde |
| CN104447242B (en) * | 2013-09-12 | 2016-05-18 | 中国科学院大连化学物理研究所 | A kind of method of preparing anhydrous formaldehyde |
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