CN102688726A - Equipment and technology for preparing furfuryl alcohol by liquid phase hydrogenation of furfural - Google Patents
Equipment and technology for preparing furfuryl alcohol by liquid phase hydrogenation of furfural Download PDFInfo
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- CN102688726A CN102688726A CN2012101723140A CN201210172314A CN102688726A CN 102688726 A CN102688726 A CN 102688726A CN 2012101723140 A CN2012101723140 A CN 2012101723140A CN 201210172314 A CN201210172314 A CN 201210172314A CN 102688726 A CN102688726 A CN 102688726A
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Abstract
The invention relates to equipment and technology for preparing furfuryl alcohol by liquid phase hydrogenation of furfural. The equipment comprises a tubular reactor with a jacket, wherein a cooling medium flows through the jacket, at least one section of supported granular catalyst blocks are filled in the tubular reactor, and the outlet of the tubular reactor is connected with a synthesized liquid storage tank. The technology comprises the steps as follows: furfural and hydrogen are preheated and pumped in the tubular reactor from the bottom; the reaction temperature is kept at 180-250 DEG C; under catalytic action of the supported granular catalyst, the retention time of the reaction is 10-90 minutes; and input amount of the hydrogen is arranged in the way of ensuring 2.0-10.0 MPa of reaction pressure. The equipment and the technology reduce consumption of catalyst greatly, and avoid the problems that traditional catalyst fine powder is hard to separate, and the prepared furfuryl alcohol is low in yield and poor in quality.
Description
Technical field
The present invention relates to a kind of equipment and technology for preparing furfuryl alcohol, belong to technical field of organic synthesis.
Background technology
Furfuryl alcohol is a kind of important Organic Chemicals.Be mainly used in and produce furfural resin, furane resins, furfuryl alcohol-pollopas, phenolic resins etc.Also be used to prepare tartaric acid, plasticizer, solvent and rocket fuel etc.In addition, also have been widely used at industrial departments such as dyestuff, synthetic fibers, rubber, agricultural chemicals and castings.
At present, the commercial production of furfuryl alcohol basically all is to adopt the preparation technology of furfural liquid-phase hydrogenatin, and employed catalyst all is the attritive powder about 300 orders.This catalyst fully mixes the back with furfural and gets into the bottom of hydrogen from tubular reactor, and reaction finishes, and catalyst and product flow out from the top of reactor.Catalyst in the final synthetic liquid is through natural subsidence or filter the formation dead catalyst.This technology is that raw material prepares furfuryl alcohol continuously in the presence of supported catalyst with furfural and hydrogen, and its reaction equation is:
The method of the preparing furfuryl alcohol by furfural liquid phase hydrogenation of Chinese patent CN101353335A adopts a complete mixing flow reactor and a plurality of piston flow reactor tandem process; It is employed to be traditional attritive powder catalyst, therefore unavoidably has drawbacks such as catalyst and consumption of raw materials height.
Though employing preparation by furfural gas phase hydrogenation such as Chinese patent CN1978051A, CN101423505A, CN1256965A are equipped with the method for furfuryl alcohol in addition; This technology need not to relate to catalyst separation, but aspects such as this technology unit efficiency and catalyst activity all have certain inferior position than liquid phase method.
Summary of the invention
The equipment and the technology that the objective of the invention is to overcome the prior art deficiency and a kind of preparing furfuryl alcohol by furfural liquid phase hydrogenation is provided, both catalytic efficiency is high, conversion ratio is high for this kind technology, again without separating catalyst.
The technical scheme that the present invention takes is:
A kind of equipment of preparing furfuryl alcohol by furfural liquid phase hydrogenation comprises the tubular reactor of jacketed being connected with cooling medium in the chuck, and at least one section support type beaded catalyst block is housed in the tubular reactor, the tubular reactor outlet with synthesize liquid storage tank and link to each other.
Described support type beaded catalyst block pref. cylindrical or sphere.
When multistage support type beaded catalyst block, leave the gap between support type beaded catalyst block.
Carry out the technology of preparing furfuryl alcohol by furfural liquid phase hydrogenation with the said equipment,, feed continuously from the tubular reactor bottom then furfural, hydrogen preheating under 100～180 ℃ of temperature; Feed cooling water in the reactor jacket; And the flow of adjusting cooling water, make reaction temperature constant, under the catalysis of support type beaded catalyst at 180～250 ℃; The time of staying of reaction, the feeding amount of hydrogen guaranteed that reaction pressure is 2.0～10.0MPa at 10～90 minutes.
The copper silicon type catalyst that described support type beaded catalyst block is a load Y aluminium oxide, its mass percent consists of: Cu:20～60%, Si:0～10%, O:20～50%, C:0～20%, Al:20～60%.
The copper silicon type Preparation of catalysts of load Y aluminium oxide adopts coprecipitation; Method is: according to the above ratio; Calculate the required copper nitrate of a certain amount of catalyst of preparation and the quality of sodium metasilicate; Be dissolved in respectively in ammoniacal liquor and the water (consumption of ammoniacal liquor, water gets final product to dissolving fully), add the carrier A l that handles through ball mill grinding again
2O
3In fully stir after; Regulate about pH to 6.0 with rare nitric acid; Again through deposition, aged at room temperature 20-25h, filtration, washing, 30-80 ℃ dry 1-5 hour, grinding, extruded moulding, 800 ℃ roasting 1-2 hour, obtain the granular pattern copper silicon type catalyst of load Y aluminium oxide at last.
The flow air speed of described support type beaded catalyst and reactant furfural (being the ratio of volume and flow) is about 0.2～1h
-1
It is raw material that the present invention adopts with furfural, hydrogen, and built-in supported solid beaded catalyst prepares furfuryl alcohol continuously in tubular reactor.Compare with existing technology; Directly adopt the built-in supported solid beaded catalyst of reactor to replace traditional furfuryl alcohol fine powder catalyst; Greatly reduce the consumption of catalyst, avoided the difficult separation problem of traditional fine powder catalyst, simultaneously product furfuryl alcohol yield height and quality better.
Description of drawings
Fig. 1 is a process equipment structural representation of the present invention;
Wherein, 1. tubular reactor, 2. chuck, 3. support type beaded catalyst block, 4. synthetic liquid basin.
The specific embodiment
Further specify implementation procedure of the present invention below in conjunction with embodiment, present embodiment is in order to understand the present invention better, and can not limit the present invention.
Embodiment 1
At a Φ 300mm, in the tubular reactor 1 of the jacketed of long 10m, built-in three sections supported solid beaded catalyst blocks 3 are connected with cooling water in the chuck 2, and tubular reactor 1 outlet links to each other with synthetic liquid basin 4.Wherein employed catalyst is a Φ 5mm pitchy cylindrical shape, the copper silicon type catalyst of load Y aluminium oxide, and its mass percent consists of: Cu:24%, Si:4%, O:34%, Al:38%, bulk density 1.2Kg/L.
Furfural, the hydrogen of prior preheating are added from reactor bottom continuously, feed cooling water in the reactor jacket, and regulate the flow of cooling water, make reaction temperature be substantially constant at 180 ± 10 ℃, the feeding amount of hydrogen guarantees that reaction pressure is 6.0MPa.The reactant furfural is 0.5h to the flow air speed of support type beaded catalyst volume
-1
The final analysis reactant liquor consists of: light component 0.58% (being mainly the 2-methylfuran), furfural 1.17%, furfuryl alcohol 95.62%, tetrahydrofurfuryl alcohol 0.12%, 5-methyl furfuryl alcohol 0.09%.The catalyst solid granule content only 0.012% in the reactant liquor.
At a Φ 300mm, in the tubular reactor 1 of the jacketed of long 10m, built-in three sections supported solid beaded catalyst blocks 3 are connected with cooling water in the chuck 2, and tubular reactor 1 outlet links to each other with synthetic liquid basin 4.Wherein employed catalyst is a Φ 5mm pitchy cylindrical shape, the copper silicon type catalyst of load Y aluminium oxide, and its mass percent consists of: Cu:24%, Si:4%, O:34%, Al:38%, bulk density 1.2Kg/L.
Furfural, the hydrogen of prior preheating are added from reactor bottom continuously, feed cooling water in the reactor jacket, and regulate the flow of cooling water, make reaction temperature be substantially constant at 200 ± 10 ℃, the feeding amount of hydrogen guarantees that reaction pressure is 6.0MPa.The reactant furfural is 0.5h to the flow air speed of support type beaded catalyst volume
-1
The final analysis reactant liquor consists of: light component 0.81% (being mainly the 2-methylfuran), furfural 0.16%, furfuryl alcohol 97.04%, tetrahydrofurfuryl alcohol 0.25%, 5-methyl furfuryl alcohol 0.17%.The catalyst solid granule content only 0.013% in the reactant liquor.
At a Φ 300mm, in the tubular reactor 1 of the jacketed of long 10m, built-in three sections supported solid beaded catalyst blocks 3 are connected with cooling water in the chuck 2, and tubular reactor 1 outlet links to each other with synthetic liquid basin 4.Wherein employed catalyst is a Φ 5mm pitchy cylindrical shape, the copper silicon type catalyst of load Y aluminium oxide, and its mass percent consists of: Cu:24%, Si:4%, O:34%, Al:38%, bulk density 1.2Kg/L.
Furfural, the hydrogen of prior preheating are added from reactor bottom continuously, feed cooling water in the reactor jacket, and regulate the flow of cooling water, make reaction temperature be substantially constant at 220 ± 10 ℃, the feeding amount of hydrogen guarantees that reaction pressure is 6.0MPa.The reactant furfural is 0.5h to the flow air speed of support type beaded catalyst volume
-1
The final analysis reactant liquor consists of: light component 1.47% (being mainly the 2-methylfuran), furfural 0.03%, furfuryl alcohol 96.46%, tetrahydrofurfuryl alcohol 0.37%, 5-methyl furfuryl alcohol 0.18%.The catalyst solid granule content only 0.017% in the reactant liquor.
Comparative example 1
At a Φ 300mm; In the tubular reactor of the jacketed of long 10m; The furfural of prior preheating, catalyst mix are added from reactor bottom after evenly continuously, and hydrogen feeds from reactor bottom continuously, and employed catalyst be 300 order copper silica fine powder catalyst of routine.Feed cooling water in the reactor jacket, and regulate the flow of cooling water, make reaction temperature be substantially constant at 200 ± 10 ℃, the feeding amount of hydrogen guarantees that reaction pressure is 6.0MPa.The flow of furfural is 2h to the flow air speed of reactor volume
-1
The final analysis reactant liquor consists of: light component 1.67% (being mainly the 2-methylfuran), furfural 0.08%, furfuryl alcohol 95.74%, tetrahydrofurfuryl alcohol 0.46%, 5-methyl furfuryl alcohol 0.17%.The catalyst solid granule content is 0.42% in the reactant liquor.
Claims (6)
1. the equipment of a preparing furfuryl alcohol by furfural liquid phase hydrogenation; It is characterized in that, comprise the tubular reactor of jacketed, be connected with cooling medium in the chuck; At least one section support type beaded catalyst block is housed in the tubular reactor, tubular reactor outlet with synthesize liquid storage tank and link to each other.
2. the equipment of a kind of preparing furfuryl alcohol by furfural liquid phase hydrogenation according to claim 1 is characterized in that, described support type beaded catalyst block is cylindrical or spherical.
3. the equipment of a kind of preparing furfuryl alcohol by furfural liquid phase hydrogenation according to claim 1 is characterized in that, when multistage support type beaded catalyst block, leaves the gap between support type beaded catalyst block.
4. carry out the technology of preparing furfuryl alcohol by furfural liquid phase hydrogenation with claim 1,2 or 3 described equipment, it is characterized in that, furfural, hydrogen preheating under 100～180 ℃ of temperature; Feed continuously from the tubular reactor bottom then, feed cooling water in the reactor jacket, and regulate the flow of cooling water; Make reaction temperature constant at 180～250 ℃; Under the catalysis of support type beaded catalyst, the time of staying of reaction, the feeding amount of hydrogen guaranteed that reaction pressure is 2.0～10.0MPa at 10～90 minutes.
5. the technology of preparing furfuryl alcohol by furfural liquid phase hydrogenation according to claim 4; It is characterized in that, the copper silicon type catalyst that described support type beaded catalyst block is a load Y aluminium oxide, its mass percent consists of: Cu:20～60%; Si:0～10%; O:20～50%, C:0～20%, Al:20～60%.
6. the technology of preparing furfuryl alcohol by furfural liquid phase hydrogenation according to claim 4 is characterized in that, the flow air speed of described support type beaded catalyst and reactant furfural is about 0.2～1h-1.
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| CN2012101723140A CN102688726A (en) | 2012-05-30 | 2012-05-30 | Equipment and technology for preparing furfuryl alcohol by liquid phase hydrogenation of furfural |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557804A (en) * | 2014-12-31 | 2015-04-29 | 宏业生化股份有限公司 | Method for synthesizing furfuralcohol through ultrasonic-assisted catalysis of furfural and device realizing method |
| CN105218492A (en) * | 2015-10-19 | 2016-01-06 | 河南心连心化肥有限公司 | Supergravity reactor is utilized to produce device and the production method of furfuryl alcohol |
| CN107771100A (en) * | 2015-06-09 | 2018-03-06 | 国际壳牌研究有限公司 | The preparation and use of copper-containing hydrogenation catalyst |
| CN109328108A (en) * | 2016-05-31 | 2019-02-12 | Ptt全球化学股份有限公司 | For preparing the preparation of the copper aluminum oxide catalyst and the catalyst of furfuryl alcohol by furfural |
| CN112546969A (en) * | 2020-12-07 | 2021-03-26 | 安徽贝克联合制药有限公司 | Catalytic hydrogenation continuous production device and preparation method of ritonavir intermediate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1341483A (en) * | 2001-09-11 | 2002-03-27 | 中国石油天然气股份有限公司 | Method for preparing tetrahydrofurfuryl alcohol by furfuralcohol hydrogenation and its catalyst |
| CN101463021A (en) * | 2008-02-22 | 2009-06-24 | 河南宏业化工有限公司 | Method and equipment for automatically and continuously producing furfuryl alcohol |
| CN102417494A (en) * | 2011-12-09 | 2012-04-18 | 宁夏共享集团有限责任公司 | Production method of high-purity furfuryl alcohol |
| CN202666814U (en) * | 2012-05-30 | 2013-01-16 | 山东一诺生化科技有限公司 | Equipment for preparing furfuryl alcohol by furfural liquid-phase hydrogenization method |
-
2012
- 2012-05-30 CN CN2012101723140A patent/CN102688726A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1341483A (en) * | 2001-09-11 | 2002-03-27 | 中国石油天然气股份有限公司 | Method for preparing tetrahydrofurfuryl alcohol by furfuralcohol hydrogenation and its catalyst |
| CN101463021A (en) * | 2008-02-22 | 2009-06-24 | 河南宏业化工有限公司 | Method and equipment for automatically and continuously producing furfuryl alcohol |
| CN102417494A (en) * | 2011-12-09 | 2012-04-18 | 宁夏共享集团有限责任公司 | Production method of high-purity furfuryl alcohol |
| CN202666814U (en) * | 2012-05-30 | 2013-01-16 | 山东一诺生化科技有限公司 | Equipment for preparing furfuryl alcohol by furfural liquid-phase hydrogenization method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557804A (en) * | 2014-12-31 | 2015-04-29 | 宏业生化股份有限公司 | Method for synthesizing furfuralcohol through ultrasonic-assisted catalysis of furfural and device realizing method |
| CN107771100A (en) * | 2015-06-09 | 2018-03-06 | 国际壳牌研究有限公司 | The preparation and use of copper-containing hydrogenation catalyst |
| CN105218492A (en) * | 2015-10-19 | 2016-01-06 | 河南心连心化肥有限公司 | Supergravity reactor is utilized to produce device and the production method of furfuryl alcohol |
| CN105218492B (en) * | 2015-10-19 | 2017-11-14 | 河南心连心化肥有限公司 | Utilize the device and production method of supergravity reactor production furfuryl alcohol |
| CN109328108A (en) * | 2016-05-31 | 2019-02-12 | Ptt全球化学股份有限公司 | For preparing the preparation of the copper aluminum oxide catalyst and the catalyst of furfuryl alcohol by furfural |
| CN112546969A (en) * | 2020-12-07 | 2021-03-26 | 安徽贝克联合制药有限公司 | Catalytic hydrogenation continuous production device and preparation method of ritonavir intermediate |
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Application publication date: 20120926 |