CN101070262A - Dicyclopentadiene continuous cracking novel process - Google Patents
Dicyclopentadiene continuous cracking novel process Download PDFInfo
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- CN101070262A CN101070262A CN 200710023133 CN200710023133A CN101070262A CN 101070262 A CN101070262 A CN 101070262A CN 200710023133 CN200710023133 CN 200710023133 CN 200710023133 A CN200710023133 A CN 200710023133A CN 101070262 A CN101070262 A CN 101070262A
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Abstract
This invention relates to a new style dicyclopentadiene series lytic craft. Preheat dicyclopentadiene, then enter lytic device after vaporizing to proceed lytic response; after reaction finishing, carry out separation to gain monocyclic ring pentadiene. The heating of lytic device adopts internally fired mode. This invention through change the technical process and type of heating, internal heating instead externally heating, to advance thermal efficiency, decrease slagging, and advance productive capacity. This invention could advance double productive capacity for the same heat consumption, and decoking cycle is prolonged 4 to 5 times.
Description
Technical field
The invention belongs to chemical field, being specifically related to a kind of is raw material with the dicyclopentadiene, the technology of continuous production monocycle pentadiene.
Background technology
Provado is a nicotinic insecticide of new generation, the global marketing volume reaches 1,000,000,000 U.S. dollars, China is the big country that produces and use Provado, there is family more than 20 in the producer of domestic production Provado, its operational path all is that the employing dicyclopentadiene is a starting raw material, through being cracked into the monocycle pentadiene, the monocycle pentadiene is as carrier process series reaction oneself pyridine synthesis ring, but all manufacturers all exist equipment to have high input in the production of dicyclopentadiene cracking technology, production capacity is low, coking is serious, workman's labor intensity height.
The fragmentation pattern major part of present domestic employing is: still formula cracking (see figure 1), with thermal oil as thermal barrier, this process efficiency is lower and the thermal barrier cost is also high, per three batch of materials will be changed the thermal barrier thermal oil one time, and average per three batches of yields are 88-90%, and thermal barrier consumption is also high, it is 250 kilograms that monocycle pentadiene per ton consumes thermal oil, the production cost height has increased the waste residue amount simultaneously, the uneconomical also contaminate environment of waste resource.
Secondly adopt directly outer heating pyrolyze,, use stainless steel tube as cracking tube without the thermal barrier (see figure 2), outer wall is wrapped on the vitrified pipe with nichrome wire and heats, heat is transmitted to vitrified pipe by nichrome wire and passes to cracking tube again, and this mode heat transmission resistance is big, and thermo-efficiency is low, energy is under-supply, cause yielding poorly, the cracking tube radial temperature difference is big, is much higher than the cracking tube core temperature by cracking tube wall place temperature, velocity flow profile is inhomogeneous in the cracking tube, is the major cause that causes the coking of cracking tube wall.
Summary of the invention
The objective of the invention is to overcome cracking of still formula and have a strong impact on the problem that monocycle pentadiene produce of this dual mode of outer heating pyrolyze to the existence of cracking dicyclopentadiene, through research with grope, providing a kind of has increased vapourizing unit and adopts the internal heating mode, optimized the technology of the cracking dicyclopentadiene of the rate of cleavage and the cracking residence time simultaneously on the basis of existing method.
Purpose of the present invention can reach by following measure:
A kind of dicyclopentadiene continuous cracking novel process after dicyclopentadiene preheating, vaporization, enters cracker and carries out scission reaction, separates obtaining the monocycle pentadiene after scission reaction finishes, wherein the mode that adds the thermal recovery internal heating of cracker.
Purpose of the present invention specifically can reach by following measure:
A kind of dicyclopentadiene continuous cracking novel process, with dicyclopentadiene in pre-heat vapourizer fully after the vaporization, enter and carry out scission reaction in the cracker of forming by at least two cracking tubes that communicate, the mode that adds the thermal recovery internal heating of cracking tube wherein, enter rectifying tower after the cracking of dicyclopentadiene in cracking tube finished and separate, obtain purity greater than 99% monocycle pentadiene.
Cracker preferably is made up of cracking tube that communicates and second pyrolysis pipe.Wherein the cyclopentadiene in cracking tube and the second pyrolysis pipe is by built-in heating rod heating.One time the interior temperature of reaction of cracking tube is 280～300 ℃, and the temperature of reaction in the second pyrolysis pipe is 300～320 ℃.
The residence time of dicyclopentadiene in cracker is 1～3min; The residence time in a preferred cracking tube and the second pyrolysis pipe is respectively 1～1.5min, most preferably 1min.
Temperature in the pre-heat vapourizer is 180～200 ℃.
The input speed of dicyclopentadiene can be regulated by the size of device, and the input speed of Cai Yonging is 4-6kg/min in an embodiment of the present invention.
The present invention has overcome the fixed pattern of the outer heating method of employing of the prior art, in various type of heating, select the mode that adopts internal heating with heating rod by a large amount of experiments, and change technical process, the rate of cleavage and the residence time have been regulated, make production capacity, output, serialization degree that sizable raising arranged, and reduced on the basis of coking amount, identical output and reduced energy consumption in a large number, make the present invention compared with prior art to have outstanding advantage.
After the coking of cracking tube wall, heat-transfer effect is poor on the one hand, and thermal efficiency descends, and rate of cleavage descends, and production capacity also descends, and artificial on the other hand coke cleaning has increased labour intensity, and yield is also low simultaneously.End-use device also shortens work-ing life.
The present invention carries out preheating, vaporization, a cracking, second pyrolysis, separation etc. with dicyclopentadiene and obtains high purity 99% monocycle pentadiene, and its yield and production capacity all improve.Its characteristics are:
1, change technical process, increase vapourizing unit, vaporization temperature is guaranteed to enter the dicyclopentadiene before the cracking tube and is vaporized fully at 180～200 ℃.
2, change type of heating: make internal heating into by original outer heating, temperature-stable makes the dicyclopentadiene cracking reach 80～90% at 280～300 ℃ in the cracking tube, and the second pyrolysis temperature-stable is at 300～320 ℃, the complete cracking of dicyclopentadiene that allows not cracking finish reaches more than 99%.
3, regulate the rate of cleavage and the cracking residence time, select optimum proportion, avoid on this basis or reduce coking amount.
The present invention is by change technical process and type of heating, changes internal heating into by original outer heating and improves thermo-efficiency, and the minimizing coking reaches the raising production capacity by improving thermo-efficiency, and technological operation is stable.Production capacity improves twice under the present invention and the equal heat rejection situation, and coking amount is few, and coke cleaning period prolongs original 4-5 doubly.Minimizing equipment drops into, and is easy to operate, serialization degree height.
Description of drawings
Fig. 1 is a still formula cracking dicyclopentadiene process flow sheet.
Fig. 2 is direct outer heating pyrolyze dicyclopentadiene process flow sheet.
Fig. 3 is a kind of concrete implementing process schema of the present invention.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and specific embodiment.
Embodiment 1
Concrete equipment and technical process are seen shown in Figure 3, are heated by heating rod in the cracking tube.
Equipment is selected: vaporizer is a stainless steel, heat interchanging area is 4 squares, a cracking tube electrical heating power is 30KW, the electrically heated of second pyrolysis pipe is 36KW, cracking tube is selected stainless steel 316L material diameter of phi 315 * 10mm for use, length is 2000mm, and knockout tower is 600 * 8mm for the Stainless Steel Helices diameter, and height is 8000mm.
At first dicyclopentadiene is squeezed into the dicyclopentadiene header tank with pump of constant delivery type, behind preheating carburettor temperature to 200 ℃, beginning quantitatively enters vaporizer with 5kg/min speed with dicyclopentadiene, guarantee dicyclopentadiene vaporization fully in vaporizer, enter cracking tube again one time, 285 ℃ of cracking tube temperature controls, 1～1.5 minute residence time, enter the second pyrolysis pipe again, second pyrolysis pipe temperature is controlled at 310 ℃, 1～1.5 minute residence time, enter after the cracking fully rectifying tower separate the monocycle pentadiene of purity 99%, enter monocycle pentadiene receiver, obtain the monocycle pentadiene of about 4.75kg by receiver metering per minute.
The normal operation of above-mentioned technology is opened cracking tube taking-up heating rod and is checked on the tube wall that a little black coke is arranged after 4 months, but cracking temperature and speed are not had influence substantially.
Comparative Examples 1
Concrete equipment and technical process are seen shown in Figure 2, and cracking tube is heated by heater strip.
Equipment is selected: cracking tube is selected stainless steel 316L material diameter of phi 315 * 10mm for use, length is 2000mm, on the external application ceramic jacket, electrical heating wire is 30KW around the last cracking tube electrical heating power of cracking tube, the electrically heated of second pyrolysis pipe is 36KW, knockout tower is 600 * 8mm for the Stainless Steel Helices diameter, and height is 8000mm.
At first dicyclopentadiene is squeezed into the dicyclopentadiene header tank with pump of constant delivery type, after 150 ℃ of dicyclopentadiene preheatings, beginning enters preheater with 1～2kg/min speed with dicyclopentadiene, enter cracking tube again one time, 285 ℃ of cracking tube temperature controls, 1～1.5 minute residence time, enter the second pyrolysis pipe again, second pyrolysis pipe temperature is controlled at 310 ℃, 1～1.5 minute residence time, enter after the cracking fully rectifying tower separate the monocycle pentadiene of purity 99%, enter monocycle pentadiene receiver, obtain the monocycle pentadiene of about 1.8～2.0kg by receiver metering per minute.
But it is more and more lower to change production capacity in time, and the normal operation of above-mentioned technology is after 1 month, and cracking temperature obviously descends, and the cracking production capacity descends, and opens many black cokes that cracking tube is found tube wall.
Claims (7)
1, a kind of dicyclopentadiene continuous cracking novel process, it is characterized in that after dicyclopentadiene preheating, the vaporization, enter cracker and carry out scission reaction, separate obtaining the monocycle pentadiene after reaction finishes, wherein the mode that adds the thermal recovery internal heating of cracker.
2, technology according to claim 1, it is characterized in that dicyclopentadiene in pre-heat vapourizer fully after the vaporization, enter and carry out scission reaction in the cracker of forming by at least two cracking tubes that communicate, the mode that adds the thermal recovery internal heating of cracking tube wherein, enter rectifying tower after the scission reaction of dicyclopentadiene in cracking tube finished and separate, obtain purity greater than 99% monocycle pentadiene.
3, technology according to claim 2, it is characterized in that dicyclopentadiene in pre-heat vapourizer fully after the vaporization, enter in the cracker of forming by cracking tube that communicates and second pyrolysis pipe and carry out scission reaction, wherein the dicyclopentadiene in cracking tube and the second pyrolysis pipe is by built-in heating rod heating, enter rectifying tower after the cracking of dicyclopentadiene in cracking tube finished and separate, obtain purity greater than 99% monocycle pentadiene.
4, technology according to claim 3 is characterized in that the temperature of reaction in the cracking tube is 280～300 ℃, and the temperature of reaction in the second pyrolysis pipe is 300～320 ℃.
5, technology according to claim 3 is characterized in that the residence time of dicyclopentadiene in cracker is 1～3min.
6,, it is characterized in that the residence time of dicyclopentadiene in cracking tube and second pyrolysis pipe is respectively 1～1.5min according to claim 3 or 5 described technologies.
7, technology according to claim 3 is characterized in that the temperature in the pre-heat vapourizer is 180～200 ℃.
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| CNB2007100231330A CN100537494C (en) | 2007-06-06 | 2007-06-06 | Dicyclopentadiene continuous cracking novel process |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101913977A (en) * | 2010-08-26 | 2010-12-15 | 上海立科药物化学有限公司 | Method for preparing high-purity cyclopentadiene with high yield |
| CN102442875A (en) * | 2010-10-25 | 2012-05-09 | 南通派斯第农药化工有限公司 | Preparation process for cyclopentadiene |
| CN101613248B (en) * | 2009-07-16 | 2012-09-05 | 浙江新和成股份有限公司 | Method for preparing cyclopentadiene by thermaldepolymerization of dicyclopentadiene |
| CN102707762A (en) * | 2012-06-04 | 2012-10-03 | 同济大学 | Heating power control method for waste high polymer material pyrolysis |
| CN102992939A (en) * | 2012-12-07 | 2013-03-27 | 四川大学 | High-yield preparation method for high-purity cyclopentadiene |
| CN102061185B (en) * | 2009-11-13 | 2013-10-09 | 环拓科技股份有限公司 | Successive cracking system and application thereof |
| CN103977589A (en) * | 2014-05-22 | 2014-08-13 | 濮阳惠成电子材料股份有限公司 | Continuous cracking and rectifying device |
| CN107382648A (en) * | 2017-06-28 | 2017-11-24 | 连云港埃森化学有限公司 | A kind of cyclopentadiene production technology |
| US9988324B2 (en) | 2015-11-04 | 2018-06-05 | Exxonmobil Chemical Patents Inc. | Process and system for making cyclopentadiene and/or dicyclopentadiene |
| CN111499487A (en) * | 2020-04-24 | 2020-08-07 | 青岛九祺生物工程有限公司 | Industrial production process for preparing high-purity cyclopentadiene |
-
2007
- 2007-06-06 CN CNB2007100231330A patent/CN100537494C/en active Active
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613248B (en) * | 2009-07-16 | 2012-09-05 | 浙江新和成股份有限公司 | Method for preparing cyclopentadiene by thermaldepolymerization of dicyclopentadiene |
| CN102061185B (en) * | 2009-11-13 | 2013-10-09 | 环拓科技股份有限公司 | Successive cracking system and application thereof |
| CN101913977A (en) * | 2010-08-26 | 2010-12-15 | 上海立科药物化学有限公司 | Method for preparing high-purity cyclopentadiene with high yield |
| CN102442875A (en) * | 2010-10-25 | 2012-05-09 | 南通派斯第农药化工有限公司 | Preparation process for cyclopentadiene |
| CN102707762B (en) * | 2012-06-04 | 2014-04-02 | 同济大学 | Heating power control method for waste high polymer material pyrolysis |
| CN102707762A (en) * | 2012-06-04 | 2012-10-03 | 同济大学 | Heating power control method for waste high polymer material pyrolysis |
| CN102992939A (en) * | 2012-12-07 | 2013-03-27 | 四川大学 | High-yield preparation method for high-purity cyclopentadiene |
| CN103977589A (en) * | 2014-05-22 | 2014-08-13 | 濮阳惠成电子材料股份有限公司 | Continuous cracking and rectifying device |
| CN103977589B (en) * | 2014-05-22 | 2016-01-13 | 濮阳惠成电子材料股份有限公司 | A kind of serialization cracking rectifier unit |
| US9988324B2 (en) | 2015-11-04 | 2018-06-05 | Exxonmobil Chemical Patents Inc. | Process and system for making cyclopentadiene and/or dicyclopentadiene |
| CN107382648A (en) * | 2017-06-28 | 2017-11-24 | 连云港埃森化学有限公司 | A kind of cyclopentadiene production technology |
| CN111499487A (en) * | 2020-04-24 | 2020-08-07 | 青岛九祺生物工程有限公司 | Industrial production process for preparing high-purity cyclopentadiene |
| CN111499487B (en) * | 2020-04-24 | 2021-06-04 | 黄月金 | Industrial production process for preparing high-purity cyclopentadiene |
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|---|---|
| CN100537494C (en) | 2009-09-09 |
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Effective date of registration: 20140129 Address after: 222523 Jiangsu city of Lianyungang province guannaxian heap ditch town Xingang Chemical Industrial Park Road No. 1 Patentee after: JIANGSU KESHENG CROP TECHNOLOGY CO., LTD. Address before: 224700 pearl of Jiangsu Jianhu County Road No. 888 Patentee before: Kesheng Group Co., Ltd., Jiangsu Prov. |
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