CN101544716B - Method and equipment for recycling catalyst in production of terpene resin - Google Patents

Method and equipment for recycling catalyst in production of terpene resin Download PDF

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Publication number
CN101544716B
CN101544716B CN2009100391362A CN200910039136A CN101544716B CN 101544716 B CN101544716 B CN 101544716B CN 2009100391362 A CN2009100391362 A CN 2009100391362A CN 200910039136 A CN200910039136 A CN 200910039136A CN 101544716 B CN101544716 B CN 101544716B
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fat liquid
reactor
gear
catalyzer
liquid take
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CN101544716A (en
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张乃银
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Luoding Xingguang Chemical Engineering Co., Ltd.
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张乃银
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

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Abstract

The invention discloses a method and equipment for recycling catalyst in the production of terpene resin, which is characterized in that a reaction kettle (3) is internally provided with a fat liquor guiding device (1), fat liquor which is reaction product and catalyst are layered because of density difference when standing in the reaction kettle (3) after the polyreaction is finished, the fat liquor is sent into a tubular container (1-1) to be guided by using the fat liquor guiding device (1), and the catalyst is remained in the reaction kettle (3) for recycling. The invention is additionally provided with the fat liquor guiding device (1) on the basis of the prior reaction kettle, has small investment and high profit, and has no any bad influence to the characteristics of the product produced by the normal process and the subsequent process; in addition, the invention has simple method and easy operation and can lower the production cost and reduce the environment pollution.

Description

The method and apparatus of catalyzer recycling during terpine resin is produced
Technical field
The present invention relates to a kind of method and apparatus of catalyzer recycling, relate in particular to the method and apparatus of catalyzer recycling in a kind of terpine resin production.Belong to the terpine resin production technical field.
Background technology
Terpine resin (C 10H 16) nClaim again polyterpene, industrial main employing aluminum trichloride (anhydrous) is that catalyzer, toluene or dimethylbenzene are solvent, the α-pinene in turps or the tall oil, beta-pinene etc. be as polymerization single polymerization monomer, carries out cationic polymerization and obtain under low-temperature condition in reactor.Because the singularity of polymerization mechanism needs in process of production to prevent that moisture from entering, reaction monomers, solvent and catalyst mix are carried out polyreaction together in nonhomogeneous system.After the polyreaction, in order to obtain pure polymeric reaction product fat liquid, must remove catalyzer.Because polymerisate fat liquid viscosity is large, catalyzer is rare moist strong, and moisture absorption process is supervened a large amount of hydrogen chloride gas, causes to adopt relatively difficulty of mechanical separation catalyzer process.
In the prior art, the reactor of polyreaction is comprised of spiral coil cooling tube, kettle, the kettle baiting valve bottom in the deceleration device of upper end, agitator, manhole, vision slit, feed port, the still, the fat liquid that after reaction finishes polymerization in the reactor is formed is discharged in the washing kettle by baiting valve together with catalyzer, heating water in the washing kettle again, pass into steam and stirring, carry out oily water separation after leaving standstill, fat liquid is as product-collecting, and catalyzer discharges together with waste water.Have following shortcoming: remaining catalyzer can not recycle (can only disposablely use) after (1) polyreaction, causes the catalyzer waste, has not only increased production cost, and has caused easily environmental pollution.(2) owing to need in washing kettle, to add the hot water injection and pass into steam-stirring, many, the complex process of equipment used, therefore, cause not only that water loss is large, energy consumption is high, the catalyzer consumption is high, resource utilization is low, production cost is high, and it is high to process the waste water cost of discharging.
Summary of the invention
One of purpose of the present invention, be for solve terpine resin produce in catalyst utilization low, the shortcomings such as cost for wastewater treatment height, provide terpine resin produce in the method for catalyzer recycling.
Two of purpose of the present invention has provided a kind of equipment of producing the catalyzer recycling for terpine resin.
One of purpose of the present invention can be achieved through the following technical solutions:
The method of catalyzer recycling during terpine resin is produced is characterized in that:
1) fat liquid take-up gear at first is set in reactor, the introducing port of fat liquid take-up gear is communicated with between the inner chamber middle part or bottom and middle part of reactor, and wash water valve cuts out;
2) leave standstill in reactor after the polyreaction of production terpine resin finishes, question response product fat liquid and catalyzer are because of the difference in specific gravity layering, and the upper strata is reaction product fat liquid, and lower floor is catalyzer;
3) utilize fat liquid take-up gear, the reaction product fat liquid on upper strata is sent in the tubular vessel derives, lower floor catalyzer be deposited in the reactor, until catalyzer sinks down into the bottom of reactor, wait until to produce next time and reuse.
One of purpose of the present invention can also be achieved through the following technical solutions:
One embodiment of the present invention are: the introducing port along continuous straight runs of described fat liquid take-up gear arranges, to reduce or to prevent that catalyzer from entering in the tubular vessel from introducing port.
The principle that the present invention reuses catalyzer is as follows:
Polyreaction leaves standstill for some time in reactor after finishing, and reacted mixture comprises polymeric reaction product fat liquid and catalyzer etc. because of the former thereby layering of difference in specific gravity, and catalyst sedimentation is to Polycondensation Reactor and Esterification Reactor, and the fat liquid level is in the catalyzer upper strata; Under the effect of fat liquid take-up gear, fat liquid is entered in the tubular vessel of fat liquid take-up gear by introducing port, and catalyzer still is retained in and uses when polyreaction is supplied with next time in reactor bottom, reaches the purpose of recycling.
Two of purpose of the present invention can be achieved through the following technical solutions:
Be used for terpine resin and produce the equipment of catalyzer recycling, comprise reactor and the blowdown apparatus that is arranged on the reactor bottom, described blowdown apparatus is made of blow-off pipe and wash water valve, it is characterized in that: at reactor one fat liquid take-up gear is set, the introducing port of this fat liquid take-up gear stretches in the reactor and is communicated with between the inner chamber middle part or bottom and middle part of reactor, and the export mouth of fat liquid take-up gear connects fat liquid blow-off valve.
Two of purpose of the present invention can also be achieved through the following technical solutions:
One embodiment of the present invention are: the main part of described fat liquid take-up gear is made of tubular vessel, and the export mouth of fat liquid take-up gear is the exit end of tubular vessel; The top seal of tubular vessel, the sidewall at the close top of tubular vessel arranges several through holes, and these several through holes consist of the introducing port of fat liquid take-up gears; Perhaps in the open top of tubular vessel, on this top, open top position one pipe cap is set, has the space between pipe cap and this open top, this space consists of the introducing port of fat liquid take-up gear.
One embodiment of the present invention are: described pipe cap can be made of the pipe cap with side hole, and this side hole consists of the introducing port of fat liquid take-up gear.
One embodiment of the present invention are: entered by introducing port in the tubular vessel of fat liquid take-up gear in order to prevent the catalyzer that sinks to Polycondensation Reactor and Esterification Reactor, the position of the introducing port of described fat liquid take-up gear is higher than Polycondensation Reactor and Esterification Reactor 30~40cm; Pipe cap is fixed in open-topped tubular vessel inlet end top by web member, and the pipe cap shadow area is not less than the entrance shadow area of tubular vessel.
One embodiment of the present invention are: the exit end of tubular vessel is connected with fat liquid blow-off valve by joint flange; The inlet end of blow-off pipe is communicated with reactor by the reactor flange, and the exit end of blow-off pipe is connected with wash water valve by joint flange.
One embodiment of the present invention are: described pipe cap can be fixed and open-topped tubular vessel inlet end top by two above stainless steel rod iron web members.
One embodiment of the present invention are: each integral part material of the present invention is the 316L stainless steel.
The beneficial effect that the present invention has is as follows:
1, the present invention separates recycling to catalyzer by physical method from fat liquid, and method is simple, and processing ease has save catalyst, reduces energy consumption, reduces production costs, the beneficial effect such as environmental contamination reduction.
2, on the reactor basis of device of the present invention in existing terpine resin is produced, set up fat liquid take-up gear, have that investment is little, the advantage of high efficiency, and to the character of normal explained hereafter product and following process process without features such as any adverse influences.
3, it is large after the present invention has avoided in the existing production technique polyreaction to finish fat liquid and catalyzer all to be entered the water loss that causes when washing kettle carries out oily water separation from the blow-off valve discharge of reactor bottom, is rich in the shortcomings such as cost for wastewater treatment height of catalyzer.
Description of drawings
Fig. 1 is the structural representation of equipment of the present invention in the specific embodiment.
Fig. 2 is the structural representation of equipment of the present invention in the specific embodiment.
Specific embodiment
Specific embodiment 1
Fig. 1 consists of specific embodiments of the invention 1.
The method of catalyzer recycling is 1 in the terpine resin production) at first at the reactor 3 interior fat liquid take-up gears 1 that arrange, the introducing port 1-2 of fat liquid take-up gear 1 is communicated with between the inner chamber middle part or bottom and middle part of reactor 3, and wash water valve 5 cuts out; 2) leave standstill in reactor 3 after the polyreaction of production terpine resin finishes, question response product fat liquid and catalyzer are because of the difference in specific gravity layering, and the upper strata is reaction product fat liquid, and lower floor is catalyzer; 3) utilizing fat liquid take-up gear 1 that upper strata fat liquid is sent in the tubular vessel 1-1 is derived by export mouth 1-3, and the catalyzer that lower floor is sink to reactor 3 bottoms is deposited in the reactor 3, waits until to produce next time and reuses.
Be used for terpine resin and produce the equipment of catalyzer recycling, comprise fat liquid take-up gear 1, blow-off pipe 2, reactor 3; Fat liquid take-up gear 1 is made of tubular vessel 1-1 and the introducing port 1-2 of main part, introducing port 1-2 stretches in the reactor 3 and is communicated with between the inner chamber middle part or bottom and middle part of reactor 3, and the export mouth 1-3 of fat liquid take-up gear 1 is that the exit end of tubular vessel 1-1 connects fat liquid blow-off valve 4 by joint flange 6-1; The inlet end of blow-off pipe 2 is communicated with reactor 3 by reactor flange 6-2, and the exit end of blow-off pipe 2 is connected with wash water valve 5 by joint flange 6-3.
The characteristics of present embodiment are: the top seal of described tubular vessel 1-1, the introducing port 1-2 of several through holes, formation fat liquid take-up gear is set near the sidewall at top at tubular vessel 1-1, the position of the introducing port 1-2 of described fat liquid take-up gear 1 is higher than Polycondensation Reactor and Esterification Reactor 30~40cm, prevents that the catalyzer that sinks to Polycondensation Reactor and Esterification Reactor from being entered in the tubular vessel 1-1 of fat liquid take-up gear 1 by introducing port 1-2.
Certain chemical industry company limited uses method and apparatus of the present invention in terpine resin is produced, make catalyzer add utilization ratio and reach 30%.The said firm is installed in equipment of the present invention respectively on original two 6 cubic metres in company and the 3 cubic metres of polymerization reaction kettles.In process of production, after polyreaction finishes, reaction mixture sat 10 minutes, most of catalyst precipitation is to the reactor bottom, and fat liquid enters in the tubular vessel 1-1 from introducing port 1-2, is flowed out by 4 controls of fat liquid blow-off valve to enter next production link; Catalyzer is retained in 3 ends of reactor, reuses during for next time polymerization; When production stopped, the catalyzer and other mixtures that adopting the hot water dissolving to remain in 3 ends of reactor were discharged through blow-off pipe 2 by wash water valve 5 controls.
Wherein, joint flange 6-1 must mate with fat liquid blow-off valve flange, and reactor flange 6-2 must be complementary with the discharging flange of reactor, and wash water valve joint flange 6-3 must mate with the wash water valve flange.Each integral part material of the present invention is the 316L stainless steel.
The inventive method is simple, processing ease, can reduce catalyzer blocking pipeline phenomenon, can improve the catalyzer utilising efficiency again, reduce the Non-aqueous processing cost, it is little to have investment, the benefit high, and present device is made simple simultaneously, existing installation is changed little, to the character of normal explained hereafter product and following process process without any adverse influence.
Specific embodiment 2
Fig. 2 consists of specific embodiments of the invention 2.
The characteristics of present embodiment are: the open top of described tubular vessel 1-1, on this top, top open part position one pipe cap 1-4 is set, and have the space between pipe cap 1-4 and this open top, this space consists of the introducing port 1-2 of fat liquid take-up gear.The position of described introducing port 1-2 is higher than Polycondensation Reactor and Esterification Reactor 30~40cm; Pipe cap 1-4 is fixed in open-topped tubular vessel 1-1 inlet end top by web member 1-4-1, and pipe cap 1-4 shadow area is not less than the entrance shadow area of tubular vessel 1-1.Described web member 1-4-1 can be comprised of two above stainless steel rod irons, plays the fixedly effect of pipe cap, between pipe cap 1-4 and the tubular vessel 1-1 inlet end sufficient space and space is arranged, and allows fat liquid flow in the tubular vessel 1-1.All the other are identical with specific embodiment 1.
Specific embodiment 3
The characteristics of present embodiment are: described pipe cap 1-4 is made of the pipe cap with side hole, this side hole consists of the introducing port 1-2 of fat liquid take-up gear, with between the pipe cap of side hole and the open-topped tubular vessel 1-1 inlet end space being arranged, can there be the space yet.Pipe cap 1-4 shadow area is not less than the entrance shadow area of tubular vessel 1-1.All the other are identical with specific embodiment 1.

Claims (7)

1. the method for catalyzer recycling during terpine resin is produced is characterized in that:
1) fat liquid take-up gear (1) at first is set in reactor (3), the introducing port (1-2) of fat liquid take-up gear (1) is communicated with between the inner chamber middle part or bottom and middle part of reactor (3), and wash water valve (5) cuts out;
2) leave standstill in reactor (3) after the polyreaction of production terpine resin finishes, question response product fat liquid and catalyzer are because of the difference in specific gravity layering, and the upper strata is for answering product fat liquid, and lower floor is catalyzer;
3) utilize fat liquid take-up gear (1), the reaction product fat liquid on upper strata is sent in the tubular vessel (1-1) derives, and the catalyzer of lower floor is deposited in the reactor (3), waits until to produce next time and reuses;
4) introducing port (1-2) the along continuous straight runs setting of described fat liquid take-up gear (1) is to reduce or to prevent that catalyzer from entering in the tubular vessel (1-1) from introducing port (1-2).
2. be used for the equipment that terpine resin is produced the catalyzer recycling, comprise reactor (3) and be arranged on the blowdown apparatus of reactor (3) bottom, described blowdown apparatus is made of blow-off pipe (2) and wash water valve (5), it is characterized in that: at reactor (3) a fat liquid take-up gear (1) is set, the introducing port (1-2) of this fat liquid take-up gear (1) stretches in the reactor (3) and is communicated with between the inner chamber middle part or bottom and middle part of reactor (3), and the export mouth (1-3) of fat liquid take-up gear (1) connects fat liquid blow-off valve (4); Introducing port (1-2) the along continuous straight runs setting of described fat liquid take-up gear (1) is to reduce or to prevent that catalyzer from entering in the tubular vessel (1-1) from introducing port (1-2).
3. according to claim 2ly produce the equipment of catalyzer recycling for terpine resin, it is characterized in that: the main part of described fat liquid take-up gear (1) is made of tubular vessel (1-1); The export mouth (1-3) of fat liquid take-up gear (1) is the exit end of tubular vessel (1-1); The top seal of tubular vessel (1-1), the introducing port (1-2) of several through holes, formation fat liquid take-up gear (1) is set near the sidewall at top at tubular vessel (1-1), perhaps in the open top of tubular vessel (1-1), on this top, open top position one pipe cap (1-4) is set, have the space between pipe cap (1-4) and this open top, described space consists of the introducing port (1-2) of fat liquid take-up gear (1).
4. according to claim 3ly produce the equipment of catalyzer recycling for terpine resin, it is characterized in that: described pipe cap (1-4) is made of the pipe cap with side hole, and side hole consists of the introducing port (1-2) of fat liquid take-up gear (1).
5. according to claim 3ly produce the equipment of catalyzer recycling for terpine resin, it is characterized in that: the position of the introducing port (1-2) of described fat liquid take-up gear (1) is higher than Polycondensation Reactor and Esterification Reactor 30 ~ 40cm; Pipe cap (1-4) is fixed in open-topped tubular vessel (1-1) inlet end top by web member (1-4-1), and pipe cap (1-4) shadow area is greater than the entrance shadow area of tubular vessel (1-1).
6. according to claim 2ly produce the equipment of catalyzer recycling for terpine resin, it is characterized in that: the export mouth (1-3) of fat liquid take-up gear (1) is connected with fat liquid blow-off valve (4) by joint flange (6-1); The inlet end of blow-off pipe (2) is communicated with reactor (3) by reactor flange (6-2), and the exit end joint flange (6-3) of blow-off pipe (2) is connected with wash water valve (5).
7. according to claim 5ly produce the equipment of catalyzer recycling for terpine resin, it is characterized in that: described web member (1-4-1) is made of two above stainless steel rod irons.
CN2009100391362A 2009-05-04 2009-05-04 Method and equipment for recycling catalyst in production of terpene resin Expired - Fee Related CN101544716B (en)

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CN2009100391362A CN101544716B (en) 2009-05-04 2009-05-04 Method and equipment for recycling catalyst in production of terpene resin

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CN2009100391362A CN101544716B (en) 2009-05-04 2009-05-04 Method and equipment for recycling catalyst in production of terpene resin

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CN101544716B true CN101544716B (en) 2013-03-20

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1631916A (en) * 2004-11-21 2005-06-29 蓝运泉 Production method of terpene resin
CN1709927A (en) * 2005-07-08 2005-12-21 广西大学 Method for preparing colorless terpene resin

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1631916A (en) * 2004-11-21 2005-06-29 蓝运泉 Production method of terpene resin
CN1709927A (en) * 2005-07-08 2005-12-21 广西大学 Method for preparing colorless terpene resin

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Effective date of registration: 20160419

Address after: Shuang Dong Zhen Bai He Dun Cun 527200 Guangdong city of Luoding Province

Patentee after: Luoding Xingguang Chemical Engineering Co., Ltd.

Address before: 527200 Guangdong Province, Luoding City Shuang Dong Zhen Bai He Dun Cun Guang Chemical Co.

Patentee before: Zhang Naiyin

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Granted publication date: 20130320

Termination date: 20180504