CN1261399C - Preparation method for isopentyl aldehyde - Google Patents
Preparation method for isopentyl aldehyde Download PDFInfo
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- CN1261399C CN1261399C CNB031292003A CN03129200A CN1261399C CN 1261399 C CN1261399 C CN 1261399C CN B031292003 A CNB031292003 A CN B031292003A CN 03129200 A CN03129200 A CN 03129200A CN 1261399 C CN1261399 C CN 1261399C
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- isoamyl alcohol
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Abstract
The present invention relates to a method for preparing isopentyl aldehyde by using isoamyl alcohol as initial raw material. A method for preparing isopentyl aldehyde by using an Ag/KZSM-5 molecular sieve as a catalyst exists with very large potential safety hazard, the catalyst has the disadvantages of hard preparation, high cost, short service life and high productive energy consumption, and the quantity of oxygen in the process of reaction is hard to control. The present invention is characterized in that isoamyl alcohol is heated until phenomenon of gasification occurs, and then reaction of high-temperature catalytic dehydrogenation is carried out by using brass catalysts; gas generated in the reaction is condensed and separated to obtain products of isopentyl aldehyde, and the brass catalysts are copper/zinc alloys, copper/tin alloys or copper/nickel alloys. The present invention can not generate corrosion to equipment besides ensuring high conversion rate and selectivity, and environmental pollution is less; additionally, the present invention has the advantages of easy preparation of catalysts, low cost, long service life and high production safety.
Description
Technical field
The present invention relates to a kind of is the method that starting raw material prepares isovaleric aldehyde with the primary isoamyl alcohol.
Background technology
Isovaleric aldehyde is raw material, the intermediate of compound essence spices and the raw material of foodstuffs industry and pharmaceutical industry of making isovaleric acid.The preparation method of isovaleric aldehyde mainly adopts oxidation style at present, with sulfuric acid, dichromic acid (salt), Cr
2O
3, MnO
2Deng primary isoamyl alcohol being oxidized to isovaleric aldehyde in liquid phase, sulfuric acid, dichromic acid (salt) are serious to equipment corrosion, and environmental pollution is big, and the side reaction of generation is many; Use Cr
2O
3, MnO
2Though high etc. selectivity, the catalyzer cost is higher.
Delivered one piece " research that the last primary isoamyl alcohol catalyzed oxidation of Ag/KZSM-5 is an isovaleric aldehyde " on the 27th volume the 4th phase (1998) " Guangxi chemical industry ", it discloses a kind of method for preparing isovaleric aldehyde with primary isoamyl alcohol, this method is a catalyzer with the Ag/KZSM-5 molecular sieve, under the heating hot conditions, bubbling air carries out catalyzed oxidation, this technology environmental pollution is few, transformation efficiency and selectivity height, but Preparation of Catalyst is difficult for, use precious metals ag, Preparation of Catalyst cost height, work-ing life is short, the production energy consumption height; And the oxygen amount in the reaction is wayward, and the excessive meeting of oxygen makes isovaleric aldehyde or primary isoamyl alcohol that deep oxidation at high temperature take place, even generates CO
2And H
2O.In addition, under the high temperature aerobic conditions, there is very big potential safety hazard in the limits of explosion wide ranges of primary isoamyl alcohol and isovaleric aldehyde; Simultaneously, contain a large amount of organic gas in the tail gas with excess air (oxygen) discharge, very easily blast.Under the situation that does not solve above-mentioned safety problem, aforesaid method is difficult to realize suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes prior art, a kind of preparation method who primary isoamyl alcohol is carried out the isovaleric aldehyde of high-temperature catalytic dehydrogenation with brass class catalyzer is provided, guaranteeing under high conversion and the selectivity, equipment there is not corrosion, pollute few, the production security height, the easy and long service life of Preparation of Catalyst.
Technical scheme of the present invention is such: the preparation method of isovaleric aldehyde, it is characterized in that heating primary isoamyl alcohol to vaporization, carry out the high-temperature catalytic dehydrogenation reaction with brass class catalyzer then, the gas that reaction produces obtains the product isovaleric aldehyde after condensation, separation, described brass class catalyzer is copper/zinc alloy, copper/tin alloy or copper/nickelalloy.The present invention is gas phase continuous catalysis dehydrogenation reaction, and is safe; Catalyzer of the present invention is an alloy type, and preparation is easy, and cost is low, and long service life can not produce corrosion to equipment, and is low in the pollution of the environment.The isovaleric aldehyde that the present invention obtains has high conversion and selectivity equally.
The preparation method of described isovaleric aldehyde, brass class catalyzer is netted, in the fixed-bed reactor of packing into the vaporization after primary isoamyl alcohol carry out the high-temperature catalytic dehydrogenation reaction, the specific surface area of netted catalyst is big, makes the better effects if of catalytic dehydrogenation.
The preparation method of described isovaleric aldehyde, the air speed of catalyzer is 0.3～0.5/h (air speed: the liquid bulk product that passes through the given volume catalyzer in the unit time), the input speed of primary isoamyl alcohol is 200～380ml/h, vaporization temperature is at 160～240 ℃, the temperature of reaction of catalytic dehydrogenation is at 400～500 ℃, the selectivity of the present invention's gained in above-mentioned processing range is more than 99%, and molar yield (transformation efficiency) is more than 95%.
Technology of the present invention is simple, is guaranteeing that have the following advantages: 1) catalyzer is an alloy type, is netted under high conversion and the selectivity, and specific surface area is big, and catalytic dehydrogenation is effective, long service life; 2) can not produce corrosion to equipment, low in the pollution of the environment; 3) Preparation of Catalyst is easy, and cost is low; 4) be gas phase continuous catalysis dehydrogenation reaction, the production security height is suitable for suitability for industrialized production.
Embodiment
Embodiment 1
100 gram raw material primary isoamyl alcohol (content 99%) are delivered to preheater continuously by pump and are vaporized, the control input speed is about 300ml/h, the temperature of preheater is controlled at 200 ℃, enters air speed then and is in the fixed-bed reactor of netted copper/zinc alloy of 0.45/h, is heated to 460 ℃, reaction product enters the condenser cooling, after decompression distillation separates, obtain product isovaleric aldehyde 94.3 grams, through gas chromatographic analysis, content 〉=99.0% (m/m), transformation efficiency are 96.5%.
Embodiment 2
100 gram raw material primary isoamyl alcohol (content 99%) are delivered to preheater continuously by pump and are vaporized, the control input speed is about 260ml/h, the temperature of preheater is controlled at 240 ℃, enters air speed then and is in the fixed-bed reactor of netted copper/tin alloy of 0.5/h, is heated to 480 ℃, reaction product enters the condenser cooling, after decompression distillation separates, obtain product isovaleric aldehyde 92.8 grams, through gas chromatographic analysis, content 〉=99.0% (m/m), transformation efficiency are 95%.
Embodiment 3
100 gram raw material primary isoamyl alcohol (content 99%) are delivered to preheater continuously by pump and are vaporized, the control input speed is about 330ml/h, the temperature of preheater is controlled at 180 ℃, enters air speed then and is in the fixed-bed reactor of netted copper/nickelalloy of 0.3/h, is heated to 430 ℃, reaction product enters the condenser cooling, after decompression distillation separates, obtain product isovaleric aldehyde 93.5 grams, through gas chromatographic analysis, content 〉=99.0% (m/m), transformation efficiency are 95.7%.
Claims (3)
1, the preparation method of isovaleric aldehyde, it is characterized in that heating primary isoamyl alcohol to vaporization, carry out the high-temperature catalytic dehydrogenation reaction with brass class catalyzer then, the gas that reaction produces obtains the product isovaleric aldehyde after condensation, separation, described brass class catalyzer is copper/zinc alloy, copper/tin alloy or copper/nickelalloy.
2, the preparation method of isovaleric aldehyde according to claim 1 is characterized in that described brass class catalyzer is netted, in the fixed-bed reactor of packing into the vaporization after primary isoamyl alcohol carry out the high-temperature catalytic dehydrogenation reaction.
3, the preparation method of isovaleric aldehyde according to claim 1 and 2, the air speed that it is characterized in that catalyzer is 0.3～0.5/h, the input speed of described primary isoamyl alcohol is 200～380ml/h, and vaporization temperature is at 160～240 ℃, and the temperature of reaction of catalytic dehydrogenation is at 400～500 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031292003A CN1261399C (en) | 2003-06-11 | 2003-06-11 | Preparation method for isopentyl aldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031292003A CN1261399C (en) | 2003-06-11 | 2003-06-11 | Preparation method for isopentyl aldehyde |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1566056A CN1566056A (en) | 2005-01-19 |
| CN1261399C true CN1261399C (en) | 2006-06-28 |
Family
ID=34469237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031292003A Expired - Lifetime CN1261399C (en) | 2003-06-11 | 2003-06-11 | Preparation method for isopentyl aldehyde |
Country Status (1)
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| CN (1) | CN1261399C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2221396A1 (en) * | 2008-12-31 | 2010-08-25 | Rohm and Haas Electronic Materials LLC | Lead-Free Tin Alloy Electroplating Compositions and Methods |
| CN104926631A (en) * | 2015-05-30 | 2015-09-23 | 吉林众鑫化工集团有限公司 | Method for preparing isoamyl aldehyde from 3-methyl-3-butenyl-1 alcohol |
| CN106008180A (en) * | 2016-06-02 | 2016-10-12 | 山东成泰化工有限公司 | Method for preparation of isovaleraldehyde from isoamyl alcohol |
| CN106117024A (en) * | 2016-06-27 | 2016-11-16 | 山东成泰化工有限公司 | A kind of preparation method of isovaleral |
| CN110627645B (en) * | 2018-06-25 | 2022-06-03 | 中国石油化工股份有限公司 | Production method for preparing glyoxylic acid ester from glycolate |
| CN111718247B (en) * | 2019-03-21 | 2022-08-05 | 万华化学集团股份有限公司 | Preparation method of isovaleraldehyde |
| CN113666811B (en) * | 2021-09-13 | 2024-04-30 | 盐城市春竹香料有限公司 | Method for preparing isopentyl aldehyde by continuously catalyzing isoamyl alcohol oxidation through electrolytic silver |
-
2003
- 2003-06-11 CN CNB031292003A patent/CN1261399C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1566056A (en) | 2005-01-19 |
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Owner name: SHANDONG NHU PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: ZHEJIANG XINHECHENG CO., LTD. Effective date: 20130826 Owner name: ZHEJIANG XINHECHENG CO., LTD. Effective date: 20130826 |
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Effective date of registration: 20130826 Address after: 261108, No. 99, Chang Hai street, Binhai Economic Development Zone, Victoria Square, Shandong Patentee after: SHANDONG NHU PHARMACEUTICAL Co.,Ltd. Patentee after: ZHEJIANG NHU Co.,Ltd. Address before: 312500 No. 4 Zhenjiang North Road, Chengguan County, Zhejiang, Xinchang Patentee before: ZHEJIANG NHU Co.,Ltd. |
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Granted publication date: 20060628 |