CN101538349B - Process and equipment for continuous catalytic polymerization aggregation of C9 petroleum resin - Google Patents
Process and equipment for continuous catalytic polymerization aggregation of C9 petroleum resin Download PDFInfo
- Publication number
- CN101538349B CN101538349B CN2008100846857A CN200810084685A CN101538349B CN 101538349 B CN101538349 B CN 101538349B CN 2008100846857 A CN2008100846857 A CN 2008100846857A CN 200810084685 A CN200810084685 A CN 200810084685A CN 101538349 B CN101538349 B CN 101538349B
- Authority
- CN
- China
- Prior art keywords
- tower
- polymerization
- reaction kettle
- polymerization reaction
- solvent
- 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.)
- Active
Links
Images
Landscapes
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to a process and equipment for the continuous catalytic polymerization aggregation of C9 petroleum resin. The process adopts multi-tower refining for separating and refining C9 raw materials, and adopts a continuous catalytic polymerization technique and a solvent and low polymer stripping technique for realizing automatic continuous large-scale production, wherein a stripping tower used in the stripping technique comprises two major parts, namely a distilling section and a stripping section; the distilling section is provided with a plurality of layers of fillers for better separating gas and liquid components; and the stripping section adopts a multi-stage stripping device for stripping. The process and the equipment can overcome the drawbacks in the production process of the conventional process such as uneasy stable control, high energy consumption and unstable product quality. The C9 petroleum resin produced by the process and the equipment is improved in color phase and resin softening point.
Description
Technical field
The present invention relates to a kind of production technology and equipment of C 9 petroleum resin product, particularly a kind of integrated Processes and apparatus of continuous catalysis polymerization of C 9 petroleum resin.
Technical background
20～260 of by-product ℃ of cracking distillates in the petroleum cracking are through thermal polymerization or at BF
3, AlCl
3Can obtain the Petropols of different performance Deng polymerization under the catalyst action.Petropols are widely used in fields such as coating, printing ink, adhesive and rubber, because of its have increase stickiness, cohesiveness and with the compatibility of other resins, often itself and other high polymer material blend is improved the performance of Related product.The application of China's oil resin in recent years is in the high speed development stage, and annual growth is more than 12%; According to the chemical industry newspaper, China's annual production in 2006 is 200,000 tons, and annual requirement is about 300,000 tons, imported product is high-grade private-use class Petropols, import volume increases year by year, and the breach of Petropols is very big, so the domestic petroleum production of resins has the large development space.
China developed Petropols since 1964, started late, and successively built up some small-sized process units, but because of the raw material sources instability, technical merit was low, developed slower.Domestic existing C 9 petroleum resin production technology all is the old technology of prolonging with external, adopts more original single still batch (-type) technology, reaction condition to be difficult to strict control mostly; Adopt mixing carbon nine or crude separation carbon nine as initial feed, the product form and aspect of production are dark partially and unstable; Generally adopt decompression still formula evaporation technology in the desolventizing operation, but the design of the used evaporimeter of this technology difficulty relatively, polymer viscosity is big, especially poorer at evaporation later stage heat-transfer effect, cause in the evaporimeter local temperature too high, the resin form and aspect are worsened, when serious even coking.Exist production scale little owing to above reason causes most C 9 petroleum resin manufacturer, yield poorly problems such as product variety is single, quality instability.
Summary of the invention
The integrated Processes and apparatus of continuous catalysis polymerization that the purpose of this invention is to provide a kind of C 9 petroleum resin, use the deficiency that this Processes and apparatus can overcome above technology, device can be realized automation control, and product quality meets international standards, and is applicable to industrial production device.
Integrated technique of the present invention may further comprise the steps: 1, carbon nine pretreatments of raw material, raw material obtain refining purifying; 2, continuous catalysis polymerization technique, the operating parameter of reactor is controlled in strictness, has guaranteed the steady quality of naval stores; 3, enter solvent recovery tower in the polymer fluid and after the washing, enter the equipment stripper of this patent again, remove solvent and the granulation of oligomer aftershaping, obtain qualified products.
Concrete step is as follows:
1. carbon nine pretreatments of raw material
The accessory substance C 9 fraction of producing ethene with petroleum cracking is that raw material carries out the rectifying preliminary treatment.Mainly utilize three fractionating columns (comprise rectifying column, knockout tower and carry and heat up in a steamer tower) under the negative-pressure operation of vacuum 0.03～0.09MPa, to carry out rectifying, the rectifying column cat head is isolated and is entered knockout tower less than 200 ℃ cut and continue to separate and purify, and heavy ends extraction at the bottom of the tower utilizes.Knockout tower adopts the side direction discharging to enter to carry to heat up in a steamer tower, and side direction extraction temperature is put forward the gas phase part of heating up in a steamer tower and returned knockout tower from cat head at 80～160 ℃, heats up in a steamer tower bottom and obtains satisfactory cut and send into the continuous catalysis polymerization process from carrying.
2. continuous catalysis polymerization
Sending satisfactory light C 9 fraction here from pretreatment system sends into the polymerization reaction kettle to stablize inlet amount, add catalyst, temperature reaction behind the solvent, catalyst and solvent can join in the polymerization reaction kettle by a certain percentage, also can join in the circular route, catalyst amount is 0.1～5.0% of carbon nine raw material quality, solvent and carbon nine raw material mass ratioes 1: 1～5: 1, adopt polymerization reaction kettle external jacket and polymerization reaction kettle outer loop to force the mode of cooling to control polymeric reaction temperature, the temperature of polymerization reaction kettle is controlled between 5～70 ℃, under normal pressure～0.5MPa, carry out polymerisation, after reaching a certain height, first polymerization reaction kettle liquid level stops charging, carry out isothermal reaction after 3～6 hours, beginning is controlled material carbon nine to the polymerization reaction kettle continuous feed, the inlet amount of catalyst and solvent is carried out the continuous catalysis polymerisation.The liquid level of polymerization reaction kettle is controlled at 70%～100%, after the liquid level of first polymerization reaction kettle reaches overflow height, enter second polymerization reaction kettle, trimerization reactor successively by circulating pump at the bottom of overflow or the still, send at last and postpone still continuation polymerization, postpone still and take external jacket and still outer loop to force the mode of cooling to control polymerization temperature, process control parameter is identical with polymerization reaction kettle or close.
Described catalyst is a lewis acid catalyst, and commonly used have alchlor, alchlor, boron trifluoride and a various complex compound, and complexing agent has phenol, aliphatic carboxylic acid, aldehyde, ether, alkyl aluminum etc. in the complex compound; Preferred catalyst is boron trifluoride etherate (BF
3Et
2O).
Described solvent is one or more the mixture in benzene,toluene,xylene, n-hexane, cyclohexane, dimethyl cyclohexane, ethyl cyclohexane, pentane, normal heptane, benzinum or the mineral oil.
Described polymerization reaction kettle can be one or more series connection.Second later polymerization reaction kettle do not add raw material, and catalyst and solvent can add or not add; Described delay still does not add raw material, catalyst and solvent.
3. Petropols precipitation, stripping, granulation
Polymer fluid enters solvent recovery tower and carries out solvent recovery after neutralization washing (adopting soda lye wash commonly used to remove catalyst with washing in the described polymer fluid) sedimentation, the solvent recovery tower temperature is controlled at 120～200 ℃, tower top pressure is controlled at vacuum 0.02～0.08MPa, light components such as the solvent of recovered overhead carry out recycling, resin liquid at the bottom of the tower enters stripper, utilize superheated steam to carry out coupling vacuum stripping, stripped vapor inlet temperature 〉=210 ℃, tower top pressure control vacuum is at 0.060～0.092MPa, column bottom temperature is controlled at 150～300 ℃, the water vapour that will have oligomer steams from cat head continuously, and the qualified resin liquid behind the stripping is discharged at the bottom of the tower and sent into make-up machine granulation packing continuously.
Described stripper comprises fractionation section and stripping section two large divisions, stripper has capping (29) and back cover (19) respectively in two ends up and down, gas vent (30) is arranged in the capping (29), discharging opening (18) is arranged on the back cover, and the fractionation section is made up of packing layer (25), withdrawing fluid distributor (26), backflow accumulator (27) and demist section (28); Stripping section is made up of heat(ing) coil (37), one or more levels stripper plant, feed pipe (31), downspout (22), manhole (34).
Be provided with heat(ing) coil in～two group (37) in stripping section bottom, heat medium is conduction oil or water vapour, and this heat(ing) coil adopts the coiling of snake type, is made up of 5～10 coil pipes for every group; Selectablely be provided with one～secondary stripper plant in the stripping section middle and upper part, stripper plant comprises steam distributor, rises vapour plate, Steam Pipe.Steam distributor is an annular, outwards is symmetrically distributed at the central axis of tower, and uniform several Ф 2～6mm apertures that has on steam distributor, perforate is downward; Be provided with the circular vapour plate that rises in the bottom of steam distributor, rise vapour plate center and be provided with a Steam Pipe that makes progress, rise the vapour panel edges and be connected with tower body; Steam Pipe communicates with the stripper cavity, and the diameter of Steam Pipe is 1/10～1/5 with the diameter of tower body ratio, and the height of Steam Pipe is 1/8～1/5 of a stripping section height; The one-level stripper plant comprises that one-level steam distributor 23, one-level rise vapour plate 33 and one-level Steam Pipe 24, the secondary stripper plant comprises that second steam distributor 20, secondary rise vapour plate 36 and secondary Steam Pipe 21, one-level rises the vapour plate and secondary rises the vapour plate apart from being 1/10～1/5 of stripping section height, be provided with a downspout (22) between a secondary stripper plant, downspout (22) diameter is 100～250mm; The discharging opening of feed pipe (31) is on one-level steam distributor (23) top; On the back cover (19) of tower body liquid outlet opening (18) is arranged, this liquid outlet opening communicates with the tower body inner chamber.
Adopt the stripper of said structure can reach following effect:
1, there is the multilayer filler to separate the resin liquid of carrying secretly the steam stripped gas and steam in fractionation section design, can better separates the gas-liquid component, reach good separating effect, improve separative efficiency, improve the yield of resin liquid from stripping section;
2, stripping section adopts multistage stripper plant stripping, and every grade of stripper plant is provided with steam distributor, rises vapour plate and Steam Pipe structure.Resin liquid enters one-level stripper plant in the tower, superheated steam flows and the abundant contact heat-exchanging stripping of resin liquid raw material after the one-level steam distributor evenly distributes from bottom to top, volatilize the oligomer component in the resin liquid and enter the fractionation section in company with steam, overflow enters the secondary stripper plant after liquid phase part in the resin liquid reaches the downspout height, this design has increased the flash distillation contact heat-exchanging time of superheated steam and resin liquid, has improved the flash distillation effect; Resin liquid makes through secondary stripper plant stripping that oligomer further separates in the resin liquid; Gas phase partly enters the fractionation section through the one-level Steam Pipe behind the secondary stripping, liquid phase part enters in the cavity of stripping section bottom by the overflow of secondary Steam Pipe, again through after the heat(ing) coil of tower body heats down, the light component of small part wherein and oligomer can flash to gas again and enter fractionation section filler part by Steam Pipe, play the purpose of further separation, make flash distillation more complete.
Like this through containing a spot of light component and oligomer in the resin liquid of multi-stage separation, the transparency height of Petropols not only, glossiness is good, and softening point is improved.
Beneficial effect of the present invention:
1. the present invention adopts that multitower is refining, the discharging of knockout tower side direction, carries and heat up in a steamer tower and continue to put forward the special purified technology of heating up in a steamer purifying, can make with extra care the separation C 9 fraction, improves product yield, and the stable polymerization reaction reduces catalyst consumption;
2. adopt the continuous catalysis polymerization technique, technological parameter control is steady, constant product quality; Automation control can adapt to need of industrial production;
3. adopt stripper technology, heat-transfer effect is good; Material time of staying in system is short, has improved the form and aspect of resin; And the separating effect of resin liquid improves, and the softening point of resin is improved.Avoid still formula flash vessel the evaporation later stage because of the heat-transfer effect difference causes in the evaporimeter local temperature too high, cause the resin form and aspect to worsen, when serious even phenomenon of coking.Adopt this invention can make molding procedure flue dust index meet the occupational health standard.
4. adopt technology of the present invention and equipment can realize suitability for industrialized production, it is low to have the rig consumption energy consumption, and production control is steady, good quality of product, can overcome that the traditional handicraft production scale is little, production process is difficult for stable control, energy consumption material consumption height, the shortcoming of unstable product quality.
Description of drawings
Fig. 1 is the technological process of production of C 9 petroleum resin
Among the figure 1, cracking carbon nine head tanks 2, rectifying column 3, rectifying column condenser
4, knockout tower 5, separation column condenser 6, carry and heat up in a steamer tower
7, polymerization reaction kettle 8, delay still
9, cycle heat exchange device 10 at the bottom of the polymeric kettle, postpone cycle heat exchange device at the bottom of the still
11, catalyst storage tank 12, washing still 13, settling tank
14, solvent recovery tower 15, stripper 16, resin flow container 17, make-up machine
Fig. 2 is the stripper structure chart with two-stage gas device
Among the figure 18, discharging opening 19, back cover 20, second steam distributor 21, secondary Steam Pipe
22, downspout 23, one-level steam distributor 24, one-level Steam Pipe 25, packing layer
26, withdrawing fluid distributor 27, backflow accumulator 28, demist section 29, capping
30, gas vent 31, feed pipe 32, one-level steam inlet 33, one-level rise the vapour plate
34, manhole 35, second steam import 36, secondary rise vapour plate 37, heat(ing) coil
The specific embodiment
The invention will be further described to contrast accompanying drawing with embodiment below, rather than limit range of application of the present invention.
Embodiment 1
1, carbon nine pretreatment of raw material systems
Cracking carbon nine is through cracking carbon nine head tanks 1, with 2～7 tons of/hour feed rates to rectifying column 2 chargings, the rectifying of rectifying column negative pressure, tower top pressure is controlled at vacuum 0.03～0.05MPa, the tower overhead gas phase component is in rectifying column condenser 3 condensation rear section backflow rectifying columns, part enters knockout tower 4, separates the extraction utilization after separation column condenser 5 condensations of cat head light component; Knockout tower control tower temperature is between 50～180 ℃; The top vacuum degree is controlled at 0.05～0.08MPa, the light carbon nine of knockout tower side line extraction enters to carry and heats up in a steamer tower 6,80～160 ℃ of side direction extraction temperature controls, aperture by side direction extraction valve and carry heat up in a steamer tower at the bottom of produced quantity tower is steadily controlled, the control column bottom temperature is 100～150 ℃, put forward the gas phase part of heating up in a steamer tower and send back to the knockout tower, carry and heat up in a steamer satisfactory carbon nine raw materials of extraction at the bottom of the Tata from cat head.
2, continuous catalysis polymerization
After starting the polymerization reaction kettle feed pump and in polymerization reaction kettle 7, adding 9 1～3 tons in light carbon, start stirring arm, and circulate at the bottom of setting up still, and proportionally in polymerization reaction kettle, add catalyst and solvent, in polymerization reaction kettle 7, add catalyst 10～20kg through catalyst storage tank 11, in polymerization reaction kettle, add 1～2 ton of solvent, regulate the aperture of cycle heat exchange device 9 cooling medium control valves at the bottom of chuck and the polymeric kettle simultaneously, the reaction temperature of polymerization reaction kettle is remained between 5～70 ℃, pressure is controlled between normal pressure～0.5MPa, behind the constant temperature 3～6 hours, in polymerization reaction kettle, add raw material continuously, catalyst and solvent carry out the continuous catalysis polymerisation, control carbon nine polymerizable raw material reactors are stablized inlet amount, catalyst, solvent and carbon nine raw materials add in the ratio of inlet amount, control catalyst addition is 0.1～5.0% of carbon nine raw material quality, solvent and carbon nine raw material mass ratioes 1: 1～5: 1, the control temperature and pressure carries out polymerisation in the scope that requires, after the liquid level in the polymerization reaction kettle is higher than overflow line, send into and postpone in the still 8, in postponing still, continue polymerisation, the reaction temperature that postpones still is controlled between 5～80 ℃, by cycle heat exchange device 10 its reaction temperatures of control at the bottom of postponing the still chuck and postponing still.
3, Petropols precipitation, stripping, granulation
Polymer fluid is in washing still 12 and settling tank 13 and enter solvent recovery tower 14 after the washing sedimentation and carry out solvent recovery, the solvent recovery tower temperature is controlled at 120～200 ℃, tower top pressure is controlled at vacuum 0.02～0.08MPa, light components such as the solvent of recovered overhead carry out recycling, tower still resin liquid enters stripper 15, utilize superheated steam to carry out coupling vacuum stripping, the stripped vapor inlet temperature is necessary 〉=and 210 ℃, tower top pressure control vacuum is at 0.060～0.092MPa, column bottom temperature is controlled at 150～300 ℃, the water vapour that will have oligomer steams from cat head continuously, qualified resin liquid is discharged at the bottom of the tower and is sent into resin flow container 16 continuously behind the stripping, sends into make-up machine 17 granulations packing again.
Claims (8)
1. stripper that is used to produce Petropols, it is characterized in that described stripper comprises fractionation section and stripping section two large divisions, stripper has capping and back cover respectively in two ends up and down, gas vent is arranged in the capping, discharging opening is arranged on the back cover, and the fractionation section is made up of packing layer, backflow accumulator, withdrawing fluid distributor and demist section; Stripping section is made up of heat(ing) coil, one or more levels stripper plant, feed pipe, downspout, manhole; Wherein, heat(ing) coil in stripping section bottom is provided with～two group, heat medium is conduction oil or water vapour, this heat(ing) coil adopts the coiling of snake type, is made up of 5～10 coil pipes for every group; Be provided with one～secondary stripper plant in the stripping section middle and upper part, stripper plant comprises steam distributor, rises vapour plate and Steam Pipe, and steam distributor is an annular, central axis at tower outwards is symmetrically distributed, the uniform aperture that has on steam distributor, the diameter in hole is 2～6mm, perforate is downward; Steam Pipe communicates with the stripper cavity, is provided with a downspout between a secondary stripper plant.
2. a kind of stripper that is used to produce Petropols according to claim 1, it is characterized in that in the described stripper plant, the diameter of Steam Pipe is 1/10～1/5 with the diameter of tower body ratio, the height of Steam Pipe is 1/5～1/8 of a stripping section height, one-level rises the vapour plate and secondary rises the vapour plate apart from being 1/10～1/5 of stripping section height, and the downspout diameter is 100～250mm; The discharging opening of feed pipe is on one-level steam distributor top; On the back cover of tower body liquid outlet opening is arranged, this liquid outlet opening communicates with the tower body inner chamber.
3. the continuous catalysis polymerization integrated technique of a C 9 petroleum resin is characterized in that may further comprise the steps:
(1), carbon nine pretreatments of raw material, raw material obtains refining purifying; (2), continuous catalysis polymerization; (3), polymer fluid enters solvent recovery tower after neutralization washing sedimentation, enter the arbitrary described stripper of claim 1-2 again, removes solvent and the granulation of oligomer aftershaping goes out qualified products;
Described step (1) comprises the steps: C 9 fraction is carried out the rectifying preliminary treatment, the cut that the rectifying column cat head is isolated less than 200 ℃ enters knockout tower continuation separation purification, heavy ends extraction at the bottom of the tower utilizes, the discharging of knockout tower employing side direction enters to carry heats up in a steamer tower, side direction extraction temperature is at 80～160 ℃, put forward the gas phase part of heating up in a steamer tower and return knockout tower, heat up in a steamer tower bottom and obtain satisfactory cut and send into the continuous catalysis polymerization process from carrying from cat head;
Described step (2) may further comprise the steps:
(I) C 9 fraction that meets the requirements after the preliminary treatment, join in the polymerization reaction kettle or add in the circular route with catalyst, solvent,, in polymerization reaction kettle, add raw material, catalyst and solvent continuously by a certain percentage and carry out the continuous catalysis polymerisation after 3～6 hours in the polymerization reaction kettle isothermal reaction;
(II) liquid level of polymerization reaction kettle is controlled at 70%～100%, after the material liquid level after the polymerization reaches overflow height, send into the delay still by circulating pump at the bottom of overflow or the still and continue polymerization, postpone still and take external jacket and still outer loop to force the mode of cooling to control polymerization temperature, process control parameter is identical with polymerization reaction kettle.
4. the continuous catalysis polymerization integrated technique of a kind of C 9 petroleum resin according to claim 3 is characterized in that may further comprise the steps:
Described continuous catalysis polymerization, material by overflow or still at the bottom of circulating pump enter the back segment operation;
Material after the polymerization at first carries out solvent recovery by solvent recovery tower after neutralization washing sedimentation, enter stripper again, remove solvent and the granulation of oligomer aftershaping goes out qualified products, stripper steam inlet temperature 〉=210 ℃, tower top pressure control vacuum is at 0.060～0.092MPa, and tower still temperature is at 150～300 ℃.
5. the continuous catalysis polymerization integrated technique of a kind of C 9 petroleum resin according to claim 3, it is characterized in that the polymerization reaction kettle described in the described step (2) can be one or more series connection, second later polymerization reaction kettle do not add raw material, and catalyst and solvent can add or not add; Described delay still does not add raw material, catalyst and solvent.
6. the continuous catalysis polymerization integrated technique of a kind of C 9 petroleum resin according to claim 3, it is characterized in that catalyst amount is 0.1～5.0% of carbon nine raw material quality in the described step (2), solvent and carbon nine raw material mass ratioes 1: 1～5: 1, take polymerization reaction kettle external jacket and polymerization reaction kettle outer loop to force the mode of cooling to control polymerization temperature between 5～70 ℃, under normal pressure～0.5MPa, carry out polymerisation.
7. the continuous catalysis polymerization integrated technique of a kind of C 9 petroleum resin according to claim 3, it is characterized in that in the step (1): knockout tower pressure all is controlled to be vacuum 0.03～0.09MPa, the discharging of knockout tower employing side direction enters to carry heats up in a steamer tower, side direction extraction temperature is at 80～160 ℃, put forward the gas phase part of heating up in a steamer tower and send back to the knockout tower, heat up in a steamer satisfactory carbon nine raw materials of extraction at the bottom of the tower from carrying from cat head.
8. the continuous catalysis polymerization integrated technique of a kind of C 9 petroleum resin according to claim 3 is characterized in that step is as follows:
(1) carbon nine pretreatments of raw material
The accessory substance C 9 fraction of producing ethene with petroleum cracking is that raw material carries out the rectifying preliminary treatment, mainly utilize three fractionating columns under the negative-pressure operation of vacuum 0.03～0.09MPa, to carry out rectifying, the cut that the rectifying column cat head is isolated less than 200 ℃ enters knockout tower continuation separation purification, heavy ends extraction at the bottom of the tower utilizes, the discharging of knockout tower employing side direction enters to carry heats up in a steamer tower, side direction extraction temperature is at 80～160 ℃, put forward the gas phase part of heating up in a steamer tower and return knockout tower, heat up in a steamer tower bottom and obtain satisfactory cut and send into the continuous catalysis polymerization process from carrying from cat head;
(2) continuous catalysis polymerization
Sending satisfactory light C 9 fraction here from pretreatment system sends into the polymerization reaction kettle with stable inlet amount, add catalyst, temperature reaction behind the solvent, catalyst and solvent can join in the polymerization reaction kettle by a certain percentage, also can join in the circular route, catalyst amount is 0.1～5.0% of carbon nine raw material quality, solvent and carbon nine raw material mass ratioes 1: 1～5: 1, adopt polymerization reaction kettle external jacket and polymerization reaction kettle outer loop to force the mode of cooling to control polymeric reaction temperature, the temperature of polymerization reaction kettle is controlled between 5～70 ℃, under normal pressure～0.5MPa, carry out polymerisation, after reaching a certain height, first polymerization reaction kettle liquid level stops charging, carry out isothermal reaction after 3～6 hours, beginning is controlled material carbon nine to the polymerization reaction kettle continuous feed, the inlet amount of catalyst and solvent is carried out the continuous catalysis polymerisation; The liquid level of polymeric kettle is controlled at 70%～100%, after the liquid level of first polymerization reaction kettle reaches overflow height, enter the polymerization reaction kettle of series connection successively by circulating pump at the bottom of overflow or the still, send at last and postpone still continuation polymerization, postpone still and take external jacket and still outer loop to force the mode of cooling to control polymerization temperature, process control parameter is identical with polymerization reaction kettle;
Described polymerization reaction kettle can be one or more series connection, and second later polymerization reaction kettle do not add carbon nine raw materials, and catalyst and solvent can add or not add; Described delay still does not add carbon nine raw materials, catalyst and solvent;
(3) Petropols precipitation, stripping, granulation
Polymer fluid enters solvent recovery tower and carries out solvent recovery after neutralization washing sedimentation, the solvent recovery tower temperature is controlled at 120～200 ℃, tower top pressure is controlled at vacuum 0.02～0.08MPa, the solvent of recovered overhead carries out recycling, and the resin liquid at the bottom of the tower enters the arbitrary described stripper of claim 1-2; Utilize superheated steam to carry out coupling vacuum stripping, stripped vapor inlet temperature 〉=210 ℃, tower top pressure control vacuum is at 0.060～0.092MPa, tower still temperature is at 150～300 ℃, the water vapour that will have oligomer steams from cat head continuously, and qualified resin liquid is discharged at the bottom of the tower and sent into make-up machine granulation packing continuously behind the stripping.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100846857A CN101538349B (en) | 2008-03-18 | 2008-03-18 | Process and equipment for continuous catalytic polymerization aggregation of C9 petroleum resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100846857A CN101538349B (en) | 2008-03-18 | 2008-03-18 | Process and equipment for continuous catalytic polymerization aggregation of C9 petroleum resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101538349A CN101538349A (en) | 2009-09-23 |
| CN101538349B true CN101538349B (en) | 2010-12-08 |
Family
ID=41121754
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100846857A Active CN101538349B (en) | 2008-03-18 | 2008-03-18 | Process and equipment for continuous catalytic polymerization aggregation of C9 petroleum resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101538349B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086251B (en) * | 2010-12-27 | 2012-08-08 | 淄博鲁华泓锦化工股份有限公司 | Continuous alkali washing method of C5 petroleum resin |
| CN102086252B (en) * | 2010-12-31 | 2012-08-22 | 淄博鲁华泓锦化工股份有限公司 | Continuous polymerization production method of petroleum resin |
| CN102702434A (en) * | 2012-06-07 | 2012-10-03 | 抚顺齐隆化工有限公司 | Method of two-stage continuous polymerization production of petroleum resin |
| CN105254810A (en) * | 2015-11-10 | 2016-01-20 | 天津大学 | Continuous production method for petroleum resin |
| CN107188997B (en) * | 2017-04-25 | 2022-02-22 | 广东新华粤树脂科技有限公司 | Method for removing C9 cold polymerized petroleum resin catalyst |
| CN112830983A (en) * | 2020-12-31 | 2021-05-25 | 华东理工大学 | Rotational flow and rotation reinforced BF of C5 petroleum resin polymerization liquid3Consumption reduction method and device |
| CN112999681A (en) * | 2021-03-26 | 2021-06-22 | 广东新华粤树脂科技有限公司 | Petroleum resin stripping process |
| CN114195913B (en) * | 2021-12-23 | 2023-08-18 | 广东鲁众华新材料有限公司 | Method for improving flash evaporation effect of carbon five petroleum resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2491450Y (en) * | 2001-07-06 | 2002-05-15 | 锡山市生物化学设备厂 | Urea stripping liquid hydrolytic stripping tower |
| CN101003602A (en) * | 2007-01-13 | 2007-07-25 | 东营市神州化工有限公司 | Technique for producing petroleum resin of carbon - 9 through continuous hot polymerization in cascade connected multiple kettles |
| CN101062965A (en) * | 2007-05-28 | 2007-10-31 | 广东省茂名华粤集团有限公司 | Method for preparing petroleum resin by cracking C9 as raw material |
-
2008
- 2008-03-18 CN CN2008100846857A patent/CN101538349B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2491450Y (en) * | 2001-07-06 | 2002-05-15 | 锡山市生物化学设备厂 | Urea stripping liquid hydrolytic stripping tower |
| CN101003602A (en) * | 2007-01-13 | 2007-07-25 | 东营市神州化工有限公司 | Technique for producing petroleum resin of carbon - 9 through continuous hot polymerization in cascade connected multiple kettles |
| CN101062965A (en) * | 2007-05-28 | 2007-10-31 | 广东省茂名华粤集团有限公司 | Method for preparing petroleum resin by cracking C9 as raw material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101538349A (en) | 2009-09-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101538349B (en) | Process and equipment for continuous catalytic polymerization aggregation of C9 petroleum resin | |
| US8721842B2 (en) | Catalytic reaction-rectification integrated process and specialized device thereof | |
| CN202808649U (en) | Systemic device for preparing polyoxymethylene dimethyl ether | |
| AU2020372526A1 (en) | Gas-liquid bubbling bed reactor, reaction system and method for synthesizing carbonate | |
| CN1137161C (en) | Process for producing copolymer | |
| CN100500718C (en) | Process for producing petroleum resin by hot polymerization | |
| CN110613946B (en) | Backpack reaction rectification equipment for synthesizing diethyl oxalate and process thereof | |
| CN103788272B (en) | A kind of method of hydrotreating containing olefines unsaturated bond polymer | |
| CN100500719C (en) | Method for preparing petroleum resin by cracking C9 as raw material | |
| CN110724025B (en) | Device and method for preparing styrene by dehydrating phenethyl alcohol | |
| CN109748791B (en) | Energy-saving method for producing dimethyl adipate | |
| CN204121793U (en) | A kind of C5 Petropols remove the device of light component | |
| CN106188400B (en) | A kind of preparation process of polystyrene multi-component copolymer high molecular material | |
| CN103724370B (en) | The processing method of phosphite ester compound is prepared in the coupling of a kind of reactive distillation | |
| CN101985419A (en) | Method for preparing ethylene glycol ethyl ether acetate | |
| CN109748790A (en) | The method for producing dimethyl adipate | |
| CN101844967A (en) | Method for preparing high-quality cardanol by using cashew nut shell oil | |
| CN214973960U (en) | Production device for preparing high-molecular polymer intermediate through esterification reaction | |
| CN102442892B (en) | Preparation method of unsaturated aldehyde by aldehyde condensation | |
| CN111689827B (en) | Device and method for preparing styrene | |
| CN109400807B (en) | Production method of petroleum resin | |
| CN208776607U (en) | Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit | |
| CN1450033A (en) | Adiabatic flash method for styrene tar oil | |
| CN115414871B (en) | Method and device for synthesizing methyl methacrylate | |
| CN114195939B (en) | Tubular reactor and thermal polymerization to C 5 /C 9 Method for copolymerizing petroleum resin |
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 |