CN101962309A - Method and device for continuously producing p-menthane by utilizing bipentene - Google Patents

Method and device for continuously producing p-menthane by utilizing bipentene Download PDF

Info

Publication number
CN101962309A
CN101962309A CN 201010285080 CN201010285080A CN101962309A CN 101962309 A CN101962309 A CN 101962309A CN 201010285080 CN201010285080 CN 201010285080 CN 201010285080 A CN201010285080 A CN 201010285080A CN 101962309 A CN101962309 A CN 101962309A
Authority
CN
China
Prior art keywords
hydrogen
gas
bed reactor
fixed
links
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN 201010285080
Other languages
Chinese (zh)
Other versions
CN101962309B (en
Inventor
何小平
李鸣放
李忠海
黎继烈
黄卫文
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HUNAN SONGYUAN CHEMICAL CO Ltd
Original Assignee
HUNAN SONGYUAN CHEMICAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HUNAN SONGYUAN CHEMICAL CO Ltd filed Critical HUNAN SONGYUAN CHEMICAL CO Ltd
Priority to CN2010102850801A priority Critical patent/CN101962309B/en
Publication of CN101962309A publication Critical patent/CN101962309A/en
Application granted granted Critical
Publication of CN101962309B publication Critical patent/CN101962309B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a method and a device for continuously producing p-menthane by utilizing bipentene. The method comprises the following steps: (1) placing a catalyst into a fixed bed reactor; replacing the air by nitrogen, preheating hydrogen, introducing the hydrogen into a gas and liquor mixer, preheating the bipentene in a liquor preheater, introducing the preheated bipentene into the gas and liquor mixer, evenly mixing in the gas and liquor mixer, and introducing into the fixed bed reactor for hydrogenation; (2) cooling the materials subjected to hydrogenation reaction; and (3) carrying out gas-liquid separation on the cooled reaction materials to obtain the menthane liquid product, returning the separated hydrogen to the fixed bed reactor for hydrogenation. The invention also comprises the device for implementing the method for continuously producing the p-menthane by utilizing the bipentene. In the invention, the traditional suspension bed intermittent process is changed into a fixed bed continuous hydrogenation production process, which is beneficial for improving the unstable state in hydrogenation production, improves the working efficiency, is convenient for adopting an automatic control system in the production process, is beneficial for reducing man-made operation deviation and is convenient for amplifying the production scale. The invention has the advantages of stable product quality, safe operation, high efficiency and low consumption.

Description

The kautschin preparation is to the continuous production method and the device of alkane in the Meng
Technical field
The present invention relates to a kind of kautschin preparation to the Meng alkane continuous production method and device.
Background technology
Kautschin is the class monocyclic terpene by product (comprising Foxlene, terpinene, Paracymene or the like, the general designation kautschin) during from afforestation product turps artificial camphor and Terpineol 350, and kautschin is most of as paint solvent at present, is worth not high.Therefore, how to develop kautschin, making more, value product is a big problem.The kautschin shortening is made alkane in the Meng, then as the spices intermediate, be reprocessed into synthetic rubber initiator or other products, can improve turps converted products added value.
At present, industrial by kautschin production to the Meng alkane have following subject matter: the problem that (1) adopts hydrogenation production technique intermittently to exist: intermittently the hydrogenation production technique is kautschin to be placed on intermittently carry out hydrogenation in the hydrogenation reaction kettle, after raw material and catalyst by proportion drop into hydrogenation reaction kettle, carry out several nitrogen, hydrogen exchange, under stirring, agitator boosts then, intensification is reacted, through a few hours reaction, after the sampling detection is qualified, could shut down discharging, recovery part is used nitrogen replacement after reacting remaining hydrogen, remove by filter catalyzer and obtain product, after reusing 3 ~ 10 times, isolated catalyzer needs to change, work-ing life is short, reclaiming often, the catalyzer mass consumption; Intermittently contact and mixing effect in order to maintain a certain amount of solution-air in the hydrogenation production, hydrogen in the hydrogenation reaction kettle has accounted for about volume of about 40%, so, just make the useful volume of hydrogenation reaction kettle descend, since intermittently the hydrogenation production technique comprise charging, nitrogen hydrogen exchange, heat up, boost, multistep operations such as hydrogenation reaction, filtration, step-down, cooling, program is numerous and diverse, length consuming time, efficient is low, the energy consumption height; Under same industrial scale, require hydrogenation reaction kettle big with relevant utility appliance volume, institute takes up space also big, and labour intensity is also big; Intermittently each reactor input and output material all will carry out gas displacement in the hydrogenation production, causes hydrogen and nitrogen to waste in a large number; Because the existence of the problems referred to above, automatization control difficulty is big in the production, and the pressure and temp instability causes the difficult control of the suitable inverse ratio of alkane in the Meng, and the less stable of quality product, industrial scale are difficult to amplify; (2) present, the problem that adopts continuous fixed bed hydrogenation technology to exist: the one, used noble metal catalyst, price height; Even if select the lower non-precious metal catalyst of price for use, but because generally only be 1 month work-ing life, the longest only about 3 months, make the production operation process become loaded down with trivial details, production cost is also higher; The 2nd, according to the Meng alkane product as spices intermediate and elastomeric purposes, think cis to the Meng alkane height then carry out aftermentioned reactive activity height, therefore in producing except requiring to alkane product yield height in the Meng, also require cis to the Meng alkane selectivity good.The 3rd, solve production process whole process using computer automation control problem.
Summary of the invention
The objective of the invention is at present be with the kautschin feedstock production to the problem that exist in the alkane production Meng, a kind of product purity height, quality is good, production safety is stable, easy to operate serialization production method and device thereof to alkane in the Meng are provided.
The present invention's kautschin preparation may further comprise the steps the continuous production method of alkane in the Meng:
(1) carries out hydrogenation: with the catalyzer fixed-bed reactor of packing into, behind the nitrogen replacement air, to send into fixed-bed reactor from the fixed-bed reactor import after the hydrogen preheating, open fixed-bed reactor heating and refrigerating unit, the fixed bed reaction actuator temperature is remained under the reaction conditions; Open charge pump, the raw material kautschin is sent into gas liquid mixer through liquid after preheating, mix with the hydrogen of sending and pass through preheating from the hydrogen basin here, mix the back at gas liquid mixer and send into fixed-bed reactor, carry out hydrogenation from fixed-bed reactor top;
Described catalyzer can be high strength particle nickel, and be 3 ~ 12 months work-ing life, and in the disposable adding fixed-bed reactor, add-on is 200kg ~ 1000kg;
The kautschin preheating temperature is 80 ℃ ~ 290 ℃; The hydrogen preheating temperature is 50 ℃ ~ 260 ℃;
The operational condition of hydrogenation is: the hydrogen flowing quantity that enters fixed-bed reactor is 800 m 3/ h ~ 1000 m 3/ h(standard state meter), the kautschin flow is 0.1 m 3/ h ~ 0.5 m 3/ h, vapour-liquid ratio (volume ratio) is 1600 ~ 10000, the hydrogenation temperature is 120 ℃ ~ 300 ℃; Hydrogenation reaction pressure is 5Mpa ~ 20Mpa;
(2) cooling: the material of finishing hydrogenation reaction comes out to enter water cooler by the fixed-bed reactor bottom and is cooled to room temperature;
(3) gas-liquid separation: enter gas-liquid separator through water cooler refrigerative material and carry out gas-liquid separation, after the gas-liquid separation, obtain alkane liquid product in the Meng; Separated hydrogen carries the new hydrogen of sending here with hydrogen gas compressor to merge by the hydrogen recycle compressor, again after the preheating of hydrogen preheater, enter gas liquid mixer with from the kautschin liquid mixing of liquor preheater, be back to fixed-bed reactor again and carry out hydrogenation.
Fixed-bed reactor bottom discharge product after gas-liquid separation, to the Meng alkane densely reach 90 ~ 98%, kautschin be hydrogenated to the Meng alkane transformation efficiency can reach 98% ~ 99.9%.
It should be noted that, before hydrogenation is stable, should be according to the transformation efficiency of kautschin in the sample of gas-liquid separator bottom discharge port sampling Detection with to the purity of alkane product in the Meng, control enters the hydrogen of fixed-bed reactor and the vapour-liquid ratio and the material feed rate of kautschin, regulates the temperature and pressure of fixed-bed reactor internal reaction.Fixed-bed reactor bottom discharge product after gas-liquid separation, to the Meng alkane concentration should reach 90 ~ 98%, kautschin be hydrogenated to the Meng alkane transformation efficiency should reach 98% ~ 99.9%.
Whole production is carried out continuously: constantly add kautschin and hydrogen mixture to fixed-bed reactor from fixed-bed reactor its top feed mouth, constantly emit alkane product in the Meng from fixed-bed reactor bottom discharge mouth, form continuous production, the full scale production process is sent to computer center by pressure, temperature, the flow sensor at each reference mark, implements the continuous production full automatic control.
Described preheating or heating thermal source can be electricity, superheated vapour or thermal oil.
The present invention's kautschin preparation is to the continuous production device of alkane in the Meng, mainly by material storaging tank, charge pump, the under meter I, the under meter II, liquor preheater, the hydrogen basin, hydrogen gas compressor, the hydrogen recycle compressor, the hydrogen preheater, gas liquid mixer, fixed-bed reactor, water cooler, gas-liquid separator, compositions such as product storage tank, the material storaging tank outlet links to each other with the charge pump import, the charge pump outlet links to each other with the under meter import, the outlet of under meter I links to each other with the liquor preheater import, import links to each other with gas liquid mixer in the liquor preheater outlet, the outlet of hydrogen basin links to each other with hydrogen gas compressor, the hydrogen gas compressor outlet links to each other with the import of under meter II, the outlet of under meter II links to each other with the import of hydrogen preheater, the outlet of hydrogen preheater links to each other with the gas liquid mixer import, the gas liquid mixer outlet links to each other with the fixed-bed reactor upper inlet, mixture outlet behind the hydrogenation of fixed-bed reactor bottom links to each other with cooler inlet, cooler outlet links to each other with the gas-liquid separator import, gas-liquid separator top hydrogen outlet links to each other with the hydrogen recycle compressor inlet by return line, the hydrogen recycle compressor outlet exports the merging back that links to each other with hydrogen gas compressor and links to each other with the hydrogen preheater by the under meter II, and gas-liquid separator bottom discharge mouth links to each other with product storage tank; Charge pump, under meter I, under meter II, liquor preheater, hydrogen basin, hydrogen gas compressor, hydrogen recycle compressor, hydrogen preheater, gas liquid mixer, fixed-bed reactor equipment are respectively arranged with temperature sensor or pressure transmitter or flow sensor, and temperature sensor, pressure transmitter and flow sensor all are connected with computer center.Pressure or temperature or the flow sensor of full scale production process parameter information by each reference mark is sent to computer center, implements the continuous production full automatic control.
Described fixed-bed reactor are preferably round shape, and its inside is provided with screen cloth, is used for fixing catalyzer, are provided with temperature sensor and pressure transmitter in the fixed-bed reactor; The fixed-bed reactor periphery is provided with the heating cooling jacket, and the import of heating cooling jacket links to each other with heating medium pipe, heat-eliminating medium pipe by an arm that valve is housed, and the heating thermal source can be electricity, superheated vapour or thermal oil.
Described gas liquid mixer can be spray and thanks formula gas liquid mixer, duct type gas liquid mixer etc., is used for the uniform mixing of hydrogen and kautschin.
Described charge pump can be reciprocal plunger high-pressure metering pump, and the transport capacity of pump is determined according to the size of throughput.
Described liquor preheater can be double-pipe exchanger, shell and tube heat exchanger or plate-type heat exchanger, and its heat interchanging area is determined by heat balance according to the size of throughput.
Described gas preheater can be double-pipe exchanger, shell and tube heat exchanger, plate-type heat exchanger or plate-fin heat exchanger, and its heat interchanging area is also determined by heat balance according to the size of throughput.
Described condenser can be tubular heat exchanger or plate-type heat exchanger, and its heat interchanging area is determined by heat balance according to the size of throughput.
Compared with prior art, the present invention has following advantage: (1) changes traditional suspension bed batch technology into fixed bed continuous hydrogenation production technique, be beneficial to and improve unsteady state in the hydrogenation production, enhance productivity, the convenient automatic control system that adopts in process of production, help reducing the manual operation deviation, make the hydrogenation production process reach the requirement of constant product quality, safe and efficient low consumption, make things convenient for industrial scale to amplify; (2) by selecting high strength particle nickel catalyzator for use, to kautschin high active of hydrogenation catalysis height, and low price, good stability, regenerability is good, reaches 6-12 month work-ing life, has solved the past because of the catalyst life weak point, in the production repeatedly more the cost that causes of catalyst changeout increase problem such as plant factor is low.
Description of drawings
Fig. 1 prepares alkane serialization in Meng production equipment structural representation for kautschin of the present invention.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1 hydrogen peroxide of the present invention is to alkane serialization in Meng production equipment embodiment
With reference to Fig. 1, the present invention's kautschin preparation to the Meng alkane continuous production device embodiment by forming by material storaging tank 1, charge pump 2, under meter I 3, liquor preheater 4, hydrogen basin 5, hydrogen gas compressor 6, hydrogen recycle compressor 7, under meter II 8, hydrogen preheater 9, gas liquid mixer 10, fixed-bed reactor 11, water cooler 12, gas-liquid separator 13, product storage tank 14; Material storaging tank 1 outlet links to each other with charge pump 2 imports, charge pump 2 outlets link to each other with 3 imports of under meter I, the outlet of under meter I 3 links to each other with liquor preheater 4 imports, 10 imports link to each other with gas liquid mixer in liquor preheater 4 outlets, 5 outlets of hydrogen basin link to each other with hydrogen gas compressor 6, hydrogen gas compressor 6 outlets link to each other with 8 imports of under meter II, 8 outlets of under meter II link to each other with 9 imports of hydrogen preheater, 10 imports link to each other 9 outlets of hydrogen preheater with gas liquid mixer, gas liquid mixer 10 outlets link to each other with fixed-bed reactor 11 upper inlet, fixed-bed reactor 11 bottoms have the mixture outlet behind the hydrogenation to link to each other with water cooler 12 imports, water cooler 12 outlets link to each other with gas-liquid separator 13 imports, gas-liquid separator 13 top hydrogen outlets have a return line, and 7 imports link to each other with the hydrogen recycle compressor, 7 outlets of hydrogen recycle compressor export the merging back that links to each other with hydrogen gas compressor 6 and link to each other with 9 imports of hydrogen preheater by under meter II 8, and gas-liquid separator 13 bottom discharge mouths link to each other with product storage tank 14.Charge pump 2, under meter
Figure 459602DEST_PATH_IMAGE001
3, under meter II 8, hydrogen preheater 9, liquor preheater 4, hydrogen basin 5, hydrogen gas compressor 6, hydrogen recycle compressor 7, gas liquid mixer 10 are respectively arranged with corresponding flow sensor, temperature sensor, be provided with temperature sensor and pressure transmitter in the fixed-bed reactor 11, all temperature sensors, pressure transmitter and flow sensor all are connected with computer center.Full scale production process parameter information is sent to computer center by pressure, temperature, the flow sensor at each reference mark, implements the continuous production full automatic control.
Described fixed-bed reactor 11 are round shape, its inside is provided with screen cloth, be used for fixing catalyzer, fixed-bed reactor 11 peripheries are provided with the heating cooling jacket, the import of heating cooling jacket links to each other with heating medium pipe, heat-eliminating medium pipe by an arm that valve is housed, and the heating thermal source can be electricity, superheated vapour or thermal oil.
Embodiment 2 is by the continuous production method operation steps embodiment that kautschin is equipped with to alkane in the Meng
(1) fixed-bed reactor 11 of at first catalyzer being packed into, behind the nitrogen replacement air, just send into fixed-bed reactor 11 from fixed-bed reactor 11 upper inlet by the hydrogen after 9 preheatings of hydrogen preheater, open the heating jacket of fixed-bed reactor 11, fixed-bed reactor 11 progressively are preheating to 120 ℃ ~ 300 ℃, open hydrogen gas compressor 6, with 800 m 3/ h ~ 1000 m 3/ h(standard state meter) hydrogen flowing quantity is delivered in the hydrogen preheater 9, and hydrogen is preheating to 50 ℃ ~ 260 ℃, opens charge pump 2 simultaneously, will be stored in raw material kautschin in the material storaging tank 1 with 0.1 m 3/ h ~ 0.5 m 3The flow of/h, deliver in the liquor preheater 4, kautschin is preheating to 80 ℃ ~ 290 ℃, again with the hydrogen after the preheating and kautschin in gas liquid mixer 10, control vapour-liquid ratio (volume ratio) is 1600 ~ 10000, after mixing, enter fixed-bed reactor 11, under 120 ℃ ~ 300 ℃ of temperature, pressure 5Mpa ~ 20Mpa condition, finish hydrogenation; (2) reaction product of coming out from fixed-bed reactor 11 bottoms enters water cooler 12, is cooled to room temperature in water cooler 12; (3) cooled mixture of reaction products enters gas-liquid separator 13, after gas-liquid separator 13 separates, obtains highly purifiedly to alkane product in the Meng, and product detects alkane concentration 90 ~ 98% in the Meng, kautschin be hydrogenated to the Meng alkane transformation efficiency reach 98% ~ 99.9%; And separated hydrogen is carried by the hydrogen recycle compressor and is sent additional new hydrogen here with hydrogen gas compressor and merge and enter the hydrogen preheater.
Catalyzer is a high strength particle nickel, and the catalyzer add-on can be 200kg~1000kg, and the hydrogen preheating temperature is 50 ℃~260 ℃, and the kautschin raw material preheating temperature is 120 ℃~300 ℃; The heating thermal source can be the mixture behind electricity, superheated vapour, thermal oil or the hydrogenation that comes out from fixed-bed reactor; Vapour-liquid ratio (volume ratio) can be 1600~3000, and the hydrogenation temperature is 120 ℃~300 ℃, and hydrogenation reaction pressure can be 5 Mpa~20 Mpa.
It should be noted that, before hydrogenation is stable, should be according to the transformation efficiency of kautschin in the sample of gas-liquid separator bottom discharge port sampling Detection with to the purity of alkane product in the Meng, control enters the hydrogen of fixed-bed reactor and the vapour-liquid ratio and the material feed rate of kautschin, regulates the temperature and pressure of fixed-bed reactor internal reaction.Fixed-bed reactor bottom discharge product after gas-liquid separation, to the Meng alkane concentration should reach 90 ~ 98%, kautschin be hydrogenated to the Meng alkane transformation efficiency should reach 98% ~ 99.9%.
Constantly add kautschin and hydrogen mixture to fixed-bed reactor 11 from fixed-bed reactor 11 its top feed mouths, constantly emit alkane product in the Meng, form continuous production from fixed-bed reactor 11 bottom discharge mouths.
Following examples are operating procedure condition embodiment, and catalyzer is high strength particle nickel, and operation steps is all identical with embodiment 2.
Embodiment 3 ~ 6
The hydrogenation temperature is controlled at 120 ℃, sets catalyzer add-on 700kg, 800kg, 900 kg, 1000kg respectively, 100 ℃ ~ 120 ℃ of hydrogen preheating temperatures, firpene preheating temperature are 100 ℃ ~ 120 ℃; Vapour-liquid ratio (volume ratio) is 2000,4000,6000,8000, and hydrogenation reaction pressure is 14 Mpa, 16 Mpa, 18 Mpa, 20 Mpa.Question response conditional stability, pinane content is respectively 94.2%, 95.1%, 96.2%, 98.0% in the sampling analysis hydrogenation product, and the transformation efficiency that firpene is hydrogenated to pinane reaches 98.4%, 99.1%, 99.2%, 99.4%.
Embodiment 7 ~ 10
The hydrogenation temperature is controlled at 140 ℃, sets catalyzer add-on 200kg, 600kg, 800kg, 1000kg respectively, 180 ℃ ~ 200 ℃ of hydrogen preheating temperatures, firpene preheating temperature are 180 ℃ ~ 200 ℃; Vapour-liquid ratio (volume ratio) is 1600,4000,7000,10000, and hydrogenation reaction pressure is 7 Mpa, 9 Mpa, 11 Mpa, 13 Mpa.Question response conditional stability, pinane content is respectively 90.7%, 95.2%, 97.5%, 98.1% in the sampling analysis hydrogenation product, and the transformation efficiency that firpene is hydrogenated to pinane reaches 98.1%, 99.2%, 99.5%, 99.9%.
Embodiment 10 ~ 13
The hydrogenation temperature is controlled at 260 ℃, and setting the catalyzer add-on respectively is 400kg, 700kg, 1000kg, and the hydrogen preheating temperature is 240 ℃ ~ 260 ℃, and the firpene raw material preheating temperature is 240 ℃ ~ 260 ℃.Vapour-liquid ratio (volume ratio) is 1600,7000,1000, and hydrogenation reaction pressure is 7 Mpa, 10 Mpa, 20Mpa.Question response conditional stability, in the sampling analysis hydrogenation product to the Meng alkane content be respectively 97.8%, 97.9%, 98.2%, kautschin be hydrogenated to the Meng alkane transformation efficiency reach 99.2%, 99.3%, 99.9%.

Claims (8)

1. the kautschin preparation is characterized in that the continuous production method of alkane in the Meng, may further comprise the steps:
(1) carries out hydrogenation: with the catalyzer fixed-bed reactor of packing into, behind the nitrogen replacement air, to send into fixed-bed reactor from the fixed-bed reactor import after the hydrogen preheating, open fixed-bed reactor heating and refrigerating unit, the fixed bed reaction actuator temperature is remained under the reaction conditions; Open charge pump, the raw material kautschin is sent into gas liquid mixer through liquid after preheating, mix with the hydrogen of sending and pass through preheating from the hydrogen basin here, mix the back at gas liquid mixer and send into fixed-bed reactor, carry out hydrogenation from fixed-bed reactor top;
Described catalyzer is a high strength particle nickel, and in the disposable adding fixed-bed reactor, add-on is 200kg ~ 1000kg;
The kautschin preheating temperature is 80 ℃ ~ 290 ℃; The hydrogen preheating temperature is 50 ℃ ~ 260 ℃;
The operational condition of hydrogenation is: entering the hydrogen flowing quantity of fixed-bed reactor, is 800 m 3/ h ~ 1000 m 3/ h(standard state meter), the kautschin flow is 0.1 m 3/ h ~ 0.5 m 3/ h, gas-liquid volume ratio are 1600 ~ 10000, and the hydrogenation temperature is 120 ℃ ~ 300 ℃; Hydrogenation reaction pressure is 5Mpa ~ 20Mpa;
(2) cooling: the material of finishing hydrogenation reaction comes out to enter water cooler by the fixed-bed reactor bottom and is cooled to room temperature;
(3) gas-liquid separation: enter gas-liquid separator through water cooler refrigerative material and carry out gas-liquid separation, after the gas-liquid separation, obtain alkane liquid product in the Meng; Separated hydrogen carries the new hydrogen of sending here with hydrogen gas compressor to merge by the hydrogen recycle compressor, again after the preheating of hydrogen preheater, enter gas liquid mixer with from the kautschin liquid mixing of liquor preheater, be back to fixed-bed reactor again and carry out hydrogenation.
2. device of continuous production method of implementing the preparation of kautschin according to claim 1 to alkane in the Meng, it is characterized in that, mainly by material storaging tank, charge pump, the under meter I, the under meter II, liquor preheater, the hydrogen basin, hydrogen gas compressor, the hydrogen recycle compressor, the hydrogen preheater, gas liquid mixer, fixed-bed reactor, water cooler, gas-liquid separator, product storage tank is formed, the material storaging tank outlet links to each other with the charge pump import, the charge pump outlet links to each other with the under meter import, the outlet of under meter I links to each other with the liquor preheater import, import links to each other with gas liquid mixer in the liquor preheater outlet, the outlet of hydrogen basin links to each other with hydrogen gas compressor, the hydrogen gas compressor outlet links to each other with the import of under meter II, the outlet of under meter II links to each other with the import of hydrogen preheater, the outlet of hydrogen preheater links to each other with the gas liquid mixer import, the gas liquid mixer outlet links to each other with the fixed-bed reactor upper inlet, mixture outlet behind the hydrogenation of fixed-bed reactor bottom links to each other with cooler inlet, cooler outlet links to each other with the gas-liquid separator import, gas-liquid separator top hydrogen outlet links to each other with the hydrogen recycle compressor inlet by return line, the hydrogen recycle compressor outlet exports the merging back that links to each other with hydrogen gas compressor and links to each other with the hydrogen preheater by the under meter II, and gas-liquid separator bottom discharge mouth links to each other with product storage tank; Charge pump, under meter I, under meter II, liquor preheater, hydrogen basin, hydrogen gas compressor, hydrogen recycle compressor, hydrogen preheater, gas liquid mixer, fixed-bed reactor equipment are respectively arranged with temperature sensor or pressure transmitter or flow sensor, and temperature sensor, pressure transmitter and flow sensor all are connected with computer controlling center.
3. device according to claim 2 is characterized in that, described fixed-bed reactor are round shape, and its inside is provided with the screen cloth that is used for fixing catalyzer, is provided with temperature sensor and pressure transmitter in the fixed-bed reactor; The fixed-bed reactor periphery is provided with the heating cooling jacket, and the import of heating cooling jacket links to each other with heating medium pipe, heat-eliminating medium pipe by an arm that valve is housed.
4. according to claim 2 or 3 described devices, it is characterized in that described gas liquid mixer is thanked formula gas liquid mixer or duct type gas liquid mixer for spray.
5. according to claim 2 or 3 described devices, it is characterized in that described charge pump is reciprocal plunger high-pressure metering pump.
6. according to claim 2 or 3 described devices, it is characterized in that described liquor preheater is double-pipe exchanger, shell and tube heat exchanger or plate-type heat exchanger.
7. according to claim 2 or 3 described devices, it is characterized in that described gas preheater is double-pipe exchanger, shell and tube heat exchanger, plate-type heat exchanger or plate-fin heat exchanger.
8. according to claim 2 or 3 described devices, it is characterized in that described condenser is tubular heat exchanger or plate-type heat exchanger.
CN2010102850801A 2010-09-19 2010-09-19 Method and device for continuously producing p-menthane by utilizing bipentene Active CN101962309B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010102850801A CN101962309B (en) 2010-09-19 2010-09-19 Method and device for continuously producing p-menthane by utilizing bipentene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010102850801A CN101962309B (en) 2010-09-19 2010-09-19 Method and device for continuously producing p-menthane by utilizing bipentene

Publications (2)

Publication Number Publication Date
CN101962309A true CN101962309A (en) 2011-02-02
CN101962309B CN101962309B (en) 2011-09-07

Family

ID=43515397

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010102850801A Active CN101962309B (en) 2010-09-19 2010-09-19 Method and device for continuously producing p-menthane by utilizing bipentene

Country Status (1)

Country Link
CN (1) CN101962309B (en)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838480A (en) * 2011-06-20 2012-12-26 逸盛大化石化有限公司 Preheating method for hydrogen gas in hydrogenation reactor
CN105669344A (en) * 2016-02-29 2016-06-15 常州大学 Method for synthesizing cis-pinane by alpha-pinene continuous catalytic hydrogenation
CN105860053A (en) * 2016-04-20 2016-08-17 南京林业大学 Method for continuously preparing end secondary amino polyether and special catalyst thereof
CN107390752A (en) * 2017-08-23 2017-11-24 南京扬子精细化工有限责任公司 A kind of real-time inspection and control system
CN108101728A (en) * 2018-01-31 2018-06-01 梧州学院 A kind of preparation method to Meng's alkane
CN108250009A (en) * 2016-12-29 2018-07-06 湖南长岭石化科技开发有限公司 To the preparation method of Meng's alkane
CN109364831A (en) * 2018-12-19 2019-02-22 上海璨谊生物科技有限公司 Gas-liquid catalytic reaction apparatus and system
CN109689194A (en) * 2016-09-09 2019-04-26 因坦斯凯姆集团有限公司 Hydrogenization method
CN111777647A (en) * 2020-07-31 2020-10-16 山东京博中聚新材料有限公司 Continuous hydrogenation production device and method for carbon-carbon double bonds in conjugated diene polymer
CN111889035A (en) * 2020-07-31 2020-11-06 山东京博中聚新材料有限公司 Continuous hydrogenation production device and production method for carbon-carbon double bonds in unsaturated polymer
CN114524723A (en) * 2022-01-29 2022-05-24 宿迁思睿屹新材料有限公司 2-hydroxy-6-naphthoic acid preparation process capable of continuous production and control device thereof
CN114751802A (en) * 2021-11-23 2022-07-15 辽宁抚清助剂有限公司 Industrial preparation method of p-menthane
CN116422244A (en) * 2023-06-13 2023-07-14 山东瑞诚化工设备有限公司 High-efficient safe type continuous hydrogenation equipment

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《林产化学与工业》 199403 刘先章等 双戊烯加工利用的研究(Ⅱ)--双戊烯氢化反应的中试研究 第109-114页 2-8 第14卷, 2 *
《林产化学与工业》 199403 刘先章等 双戊烯加工利用的研究(Ⅱ)--双戊烯氢化反应的中试研究 第110-113页 1 第14卷, 2 *

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838480A (en) * 2011-06-20 2012-12-26 逸盛大化石化有限公司 Preheating method for hydrogen gas in hydrogenation reactor
CN105669344A (en) * 2016-02-29 2016-06-15 常州大学 Method for synthesizing cis-pinane by alpha-pinene continuous catalytic hydrogenation
CN105860053A (en) * 2016-04-20 2016-08-17 南京林业大学 Method for continuously preparing end secondary amino polyether and special catalyst thereof
CN105860053B (en) * 2016-04-20 2018-08-14 南京林业大学 A kind of continuous method and its special-purpose catalyst for preparing end secondary amino group polyethers
CN109689194A (en) * 2016-09-09 2019-04-26 因坦斯凯姆集团有限公司 Hydrogenization method
CN108250009A (en) * 2016-12-29 2018-07-06 湖南长岭石化科技开发有限公司 To the preparation method of Meng's alkane
CN108250009B (en) * 2016-12-29 2020-08-07 湖南长岭石化科技开发有限公司 Preparation method of p-menthane
CN107390752A (en) * 2017-08-23 2017-11-24 南京扬子精细化工有限责任公司 A kind of real-time inspection and control system
CN108101728A (en) * 2018-01-31 2018-06-01 梧州学院 A kind of preparation method to Meng's alkane
CN109364831A (en) * 2018-12-19 2019-02-22 上海璨谊生物科技有限公司 Gas-liquid catalytic reaction apparatus and system
CN111777647A (en) * 2020-07-31 2020-10-16 山东京博中聚新材料有限公司 Continuous hydrogenation production device and method for carbon-carbon double bonds in conjugated diene polymer
CN111889035A (en) * 2020-07-31 2020-11-06 山东京博中聚新材料有限公司 Continuous hydrogenation production device and production method for carbon-carbon double bonds in unsaturated polymer
CN114751802A (en) * 2021-11-23 2022-07-15 辽宁抚清助剂有限公司 Industrial preparation method of p-menthane
CN114524723A (en) * 2022-01-29 2022-05-24 宿迁思睿屹新材料有限公司 2-hydroxy-6-naphthoic acid preparation process capable of continuous production and control device thereof
CN116422244A (en) * 2023-06-13 2023-07-14 山东瑞诚化工设备有限公司 High-efficient safe type continuous hydrogenation equipment
CN116422244B (en) * 2023-06-13 2023-10-10 山东瑞诚化工设备有限公司 High-efficient safe type continuous hydrogenation equipment

Also Published As

Publication number Publication date
CN101962309B (en) 2011-09-07

Similar Documents

Publication Publication Date Title
CN101962309B (en) Method and device for continuously producing p-menthane by utilizing bipentene
CN101962310B (en) Method for continuously producing pinane by pinene and device therefor
CN105272863B (en) The preparation method of paraphenetidine
CN101891718B (en) Continuous production process for preparing succinyl oxide by maleic anhydride hydrogenation
CN101735182A (en) Process for continuously producing succinic anhydride through hydrogenation of maleic anhydride
CN111689845B (en) Process for producing succinic acid by maleic anhydride aqueous phase hydrogenation
CN105294456B (en) The method that paraphenetidine is prepared with the device catalytic hydrogenation of industrially scalable
CN112661625A (en) Preparation process of succinic acid
CN105254484A (en) Continuous production method and device for preparing propionic acid through air oxidation of propionaldehyde
CN210787302U (en) Device for continuously producing high-purity potassium alkoxide or sodium alkoxide by using microchannel reactor
CN108499508B (en) A kind of multipoles reactors and the method for preparing cycocel using the device
CN101219920A (en) Ethanol dehydration technique adopting molecular sieve catalyst
CN207957782U (en) It is a kind of without cycle ammonia synthesis system
CN101649257B (en) Method for producing saturated oil through continuously hydrogenating castor oil and apparatus thereof
CN106831321B (en) Method and device for obtaining crude borneol by continuous saponification and stripping of borneol oxalate
CN102690163A (en) Continuous production method and device utilizing dipentene to prepare p-cymene
CN105924329B (en) Acetic acid prepares the coupling production technology of ethyl alcohol
CN218608084U (en) Suspension bed reactor for producing succinic anhydride
CN103121936B (en) Continuous malic acid synthesizing device and preparation method of malic acid
CN101049571B (en) Complex type molecular sieve catalyst, preparation method, and application in preparing crylic acid
CN202506390U (en) Reactor for producing hexanediamine through adiponitrile hydrogenation
CN106824018A (en) Shell and tube paste state bed reactor and reaction system
CN206103913U (en) Reaction unit of benzene part hydrogenation synthesis cyclohexene
CN212222830U (en) Device for preparing cyclopentene by selectively hydrogenating cyclopentadiene
CN208857167U (en) A kind of cyclohexyl benzene production system

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant