CN103275252A - Method for purification treatment on styrene polymerization recovered liquid - Google Patents
Method for purification treatment on styrene polymerization recovered liquid Download PDFInfo
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Abstract
The invention relates to a method for purification treatment on a styrene polymerization recovered liquid. The method is characterized in that through an adsorbent which is bentonite, kaolin, or one and/or more of activated clay, alumina, activated aluminum oxide, activated carbon, a molecular sieve and aluminum silicate obtained by activating treatment on bentonite and kaolin and having different particle sizes, styrene polymerization recovered liquid is purified by a layered adsorption filtration method. The method has a short process, adopts simple equipment, can be operated and controlled easily, and has good treatment effects, an impurity removal rate more than 80% and an acid value less than 0.1 after purification. The styrene polymerization recovered liquid purified by the method can be used as a solvent or a raw material and can be directly returned back to styrene polymerization or other vinyl monomer copolymerization devices.
Description
Technical field
The present invention relates to the purifying treatment method that styrene polymerization reclaims liquid, the styrene polymerization that particularly contains the impurity that equipment container produces in the monomer of the not polymerization reaction take place of separating and solvent, the production equipment from polymkeric substance reclaims the purifying treatment method of liquid.
Background technology
But known styrene monomer polymerization or will adopt letex polymerization, suspension polymerization, solution polymerization or add the bulk polymerization of a small amount of solvent during as the vinyl monomer copolymerization with the monomer of other activity polymerization reaction take places.Because vinylbenzene or other vinyl monomers itself are added with stopper, reaction process also is added with emulsifying agent, initiator, chain-transfer agent, reagent and additive in polymerization such as vinylformic acid and ester and antioxidant, the agent of interior profit, photostabilizer, dyestuff, releasing agents etc. improve the additive of product performance, therefore but reaction product is except the polymkeric substance of the monomer of vinylbenzene or vinylbenzene and other activity polymerization reaction take places, also produced small amounts of oligomer and above-mentioned reagent and additive in polymerization and additive side reaction product, the unreacted monomer of these side reaction products and part and solvent are separated the non-reacted band colored foreign that itself brings together with equipment container in the production equipment from polymkeric substance just become styrene polymerization recovery liquid.
Because the side reaction product that styrene polymerization reclaims in the liquid comprises styrene oligomer and acidity and non-acidic impurities, be transparency, the color that band color base group can influence the finished product as the phenols side reaction product for example, particularly more obvious to the influence of transparent polystyrene, also make the finished product course of processing turned to be yellow by thermooxidizing easily simultaneously; These oligopolymer and acidity or non-acidic impurities still are strong radical scavenger in addition, but thereby suppressed the polymerization of the monomer of vinylbenzene and other activity polymerization reaction take places, all adverse influence can be arranged to speed of reaction and molecular weight, and make appearance color, transparency and the mechanical property of product reduce.Above-mentioned this influence increases with the increase of impurity.Therefore these polymerizations recovery liquid are directly got back to the participation polymerization of styrene polymerization device or are had a strong impact on quality product with other vinyl monomer copolymerization meetings, can not directly use as reclaiming solvent.Patent CN 1253937 A disclose a kind of purification process of styrene monomer, mention with at least a material in aluminum oxide, activated alumina, silica gel, gac, calcium oxide and/or the pure aluminium silicate and remove phenolic compound in the styrene monomer, its technical scheme is also just removed phenylacetylene and the phenolic inhibitor in the styrene monomer, but all do not relate in the polystyrene resin production process removal of the impurity that the oligopolymer that reclaims liquid behind the styrene polymerization and side reaction impurity and production equipment equipment container self bring, and the cinnamic rate of recovery is not high.EP 410361 and EP 0662465 also only are the purifying that proposes by to styrene monomer, and remove phenylacetylene.CN 101121634 A disclose cinnamic recovery method in a kind of pyrolysis gasoline, mention and obtain raw material thing before the styrene product and select for use at least a in gac, atlapulgite or the molecular sieve to decolour as sorbent material conventional the separation, thereby the colourity of pyrolysis gasoline raw material is reduced, use precious metals palladium catalyst to carry out cinnamic recovery decolouring simultaneously.In addition, disclosed technical schemes such as lot of documents such as patent CN 102649660 A, CN 101475437 A, CN 1852877 A, CN 1087892 A are the method for removing phenylacetylene in the vinylbenzene, its principle is to impel phenylacetylene to be transformed into vinylbenzene by the method for shortening, and its crucial processing step often is the control of selection of catalysts and processing method.
Application number is 89101122.6 patent disclosure, and a kind of cracking reduction polystyrene reclaims the method for styrene monomer, its concrete technical scheme is to adopt metal oxide catalyst, place alloy additive in the cracking still bottom, high temperature carries out scission reaction, accompany by underpressure distillation simultaneously and reclaim styrene monomer, but its rate of recovery is 70 ~ 75%.Application number a kind of purification process of vi-ny l aromatic monomers that has been 91109195.5 patent disclosure, its concrete technical scheme is with the fixed bed of monomer by aluminium oxide particles, and the space velocity that limits monomer is 0.5-7.5h
-1And linear velocity is that 0.125-45m/h is to remove phenolic inhibitor.It is a kind of that application number is 95103865.6 patent disclosure is cinnamic catalyzer with the waste polystyrene plastic catalyzed degradation, its concrete technical scheme is that the Y zeolite of the special modification of employing is main component, be equipped with promotor and tackiness agent etc. under special conditions and highly active aluminium hydroxide carries out the modification processing and forms, the special compound that forms at catalyst surface makes the catalyzed degradation of polystyrene be able to carry out under the temperature of normal pressure and reduction, but the cinnamic rate of recovery only is about 60%.
Summary of the invention
For the effective elimination styrene polymerization reclaims the impurity that side reaction impurity such as oligopolymer and acid and nonacid material in the liquid and production equipment equipment container self bring, the invention provides the purifying treatment method that a kind of styrene polymerization reclaims liquid.Its technical scheme is as follows:
To be selected from wilkinite, the atlapulgite that kaolin or above-mentioned substance activation treatment become, aluminum oxide, activated alumina, gac, molecular sieve, at least a material in the pure aluminium silicate and/or the material of multiple different-grain diameter are as sorbent material, reclaiming liquid with styrene polymerization mixes by a certain percentage and carries out the layering adsorption filtration, thereby purifying treatment is removed side reaction product such as the oligopolymer that reclaims styrene polymerization in the liquid, meetings such as acidity and non-acidic impurities and production equipment equipment container itself bring influence the impurity of styrene polymerization and end product quality, obtain comparatively pure styrene polymerization and reclaim liquid.
The above-mentioned handled styrene polymerization of the present invention reclaims liquid and generally comprises following composition: styrene monomer 60 ~ 95% weight parts, but the monomer of other activity polymerization reaction take places such as vinyl monomer 0 ~ 40% weight part; Benzene class such as benzene, toluene, ethylbenzene, m-xylene, p-Xylol, o-Xylol, isopropyl benzene, n-proplbenzene and non-aromatics compound 3 ~ 30% weight parts; Oligopolymer such as vinylbenzene or other vinyl monomer polymer 1 ~ 15% weight parts; Acid and non-acidic impurities such as styrene oxidation product phenylformic acid and reagent and additive in polymerization comprise that emulsifying agent, initiator, chain-transfer agent and additive comprise the impurity of weight part 0.1 ~ 5% such as antioxidant, interior profit agent, photostabilizer, dyestuff side reaction product and micro-production equipment equipment container generation itself.But be styrene polymerization or with the monomer of other activity polymerization reaction take places such as vinyl monomer copolymerization after have above-mentioned various impurity after reaching 50 ~ 85% transformation efficiency, and from polymkeric substance, separate and become styrene polymerization and reclaim liquid.
The present invention has carried out preferably the envelope-bulk to weight ratio that above-mentioned styrene polymerization reclaims liquid and sorbent material, preferably, the envelope-bulk to weight ratio of styrene polymerization recovery liquid and sorbent material is 20 ~ 1000:1 in the described layering adsorption filtration process, more preferably, be lower than 600:1, most preferably, be lower than 300:1.
The present invention has carried out preferably the different-grain diameter of above-mentioned sorbent material, preferably, the particle diameter of described sorbent material be 0.1mm to 5.0mm, more preferably, 0.5mm is to 3mm.
The present invention has carried out preferably above-mentioned layering adsorption filtration, preferably, upper and lower two-layer be big particle diameter adsorbent layer, the middle layer is respectively the small particle size adsorbent layer of different sorbent materials.
The present invention can adopt the technical process of batch process method to realize, it is specially: the amount by styrene polymerization recovery liquid in multistage returnable adds a certain proportion of above-mentioned sorbent material respectively, styrene polymerization reclaims liquid stirring or concussion stop certain hour in returnable at different levels in order, obtain the returnable that different sorbent material purifying treatment liquid join next stage more successively by vacuum filtration, the liquid after the last step returnable is handled becomes final styrene polymerization and reclaims liquid.
The present invention has carried out preferably above-mentioned multistage returnable, and preferably, described multistage returnable is 4 grades.
The present invention has carried out preferably the envelope-bulk to weight ratio that above-mentioned batch process method styrene polymerization reclaims liquid and sorbent material, preferably, the envelope-bulk to weight ratio of styrene polymerization recovery liquid and sorbent material is 20 ~ 1000:1 in the described returnable at different levels, more preferably, be lower than 600:1, most preferably, be lower than 300:1.
The present invention can adopt the technical process of continuous online treatment method to realize, it is specially: under certain pressure and temperature styrene polymerization is reclaimed liquid and pass through a king-post continuously by certain space velocity and linear velocity, this king-post layering is filled with above-mentioned sorbent material successively, and the styrene polymerization that is purified after the processing reclaims liquid.
The present invention has carried out preferably the space velocity of above-mentioned continuous online treatment method, and preferably, described space velocity is lower than 5 h
-1, more preferably, be lower than space velocity 3 h
-1
The present invention has carried out preferably the linear velocity of above-mentioned continuous online treatment method, and preferably, described linear velocity is lower than 15 m/hr, more preferably, is lower than 8 m/hr linear velocities.
Adopt technology of the present invention that styrene polymerization is reclaimed liquid and carry out purifying treatment, can select for use styrene polymerization to reclaim the contained vinylbenzene of liquid or the oligopolymer of other vinyl monomers and this index of removal of impurity of polymerization side reactions product preferably and estimate, the acid number that also can measure the purifying treatment front and back simultaneously changes to carry out comprehensive evaluation.
The mensuration of this removal of impurity can use vapor-phase chromatography to measure the content that styrene polymerization reclaims liquid purifying treatment front and back vinylbenzene or other vinyl monomers and benzene-like compounds respectively, and is as follows:
÷ A * 100% of foreign matter content=(A-B-C)
A: styrene polymerization reclaims liquid gross weight deal (by 100 weight parts)
B: styrene polymerization reclaims vinylbenzene weight part (by 100 weight parts) in the liquid
C: the weight part of other vinyl monomers and benzene-like compounds (by 100 weight parts)
Removal of impurity %=handles foreign matter content * 100% before rear impurity content ÷ handles
The present invention compared with prior art has following outstanding advantage:
By implementing technique scheme, the present invention can effectively remove styrene polymerization and reclaim the impurity that the oligopolymer of the contained vinylbenzene of liquid or other vinyl monomers and polymerization side reactions product and production equipment equipment itself bring, adopt above-mentioned technology can make styrene polymerization reclaim removal of impurity such as the oligopolymer of contained vinylbenzene in the liquid or other vinyl monomers and polymerization side reactions product and reach more than 80%, be up to 95%; Acid number is lower than 0.1 after the purifying treatment, minimumly can reach 0.030.Simultaneously, technical process of the present invention is short, technological process is simple fast, equipment is simple and energy-conservation, can realize that on-line automatic red-tape operati, purifying treatment are respond well.The styrene polymerization of crossing through purifying treatment of the present invention reclaims liquid and can be used as solvent or raw material and directly get back to styrene polymerization or use with the copolymerization device of other vinyl monomers.
Embodiment
Below by specific embodiment the present invention is further specified, but the invention is not restricted to following examples.
Not doing the sorbent material particle diameter that specifies in following specific embodiment and the Comparative Examples is 1.5mm.
Embodiment 1, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization reclaims liquid (styrene content 81%, benzene-like compounds content 12%, the impurity equal size 7% that oligopolymer and acidity and non-acidic impurities and production equipment equipment container self bring, acid number is 0.137) to add the 25g particle diameter earlier among the 500mL be the activated alumina of 2mm, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the concussion of 25g atlapulgite as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 93% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is changed to 0.052.
Embodiment 2, styrene polymerization reclaim the purifying treatment method of liquid
Adding the 25g particle diameter earlier among the styrene polymerization recovery liquid 5000mL among the embodiment 1 is the activated alumina of 2mm, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the concussion of 25g atlapulgite as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 95% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is changed to 0.032.
Embodiment 3, styrene polymerization reclaim the purifying treatment method of liquid
Adding the 25g particle diameter earlier among the styrene polymerization recovery liquid 7000mL among the embodiment 1 is the activated alumina of 2mm, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the concussion of 25g atlapulgite as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 94% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is changed to 0.050.
Embodiment 4, styrene polymerization reclaim the purifying treatment method of liquid
Adding the 25g particle diameter earlier among the styrene polymerization recovery liquid 15000mL among the embodiment 1 is the activated alumina of 2mm, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the concussion of 25g atlapulgite as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 95% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is changed to 0.050.
Embodiment 5, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims and adds the 5g activated alumina among the liquid 5000ml earlier, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, reclaim the concussion of liquid adding 5g atlapulgite at the styrene polymerization of separating as stated above again and handle and separate, liquid removal of impurity 89% is reclaimed in the polymerization that the solution employing gas chromatograph for determination that process is filtered is purified after the processing.Acid number after the purifying treatment is 0.063.
Embodiment 6, styrene polymerization reclaim the purifying treatment method of liquid
Adding the 25g particle diameter earlier among the styrene polymerization recovery liquid 5000mL among the embodiment 1 is the activated alumina of 2mm, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the concussion of 25g activated alumina as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 80% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is changed to 0.032.
Embodiment 7, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims among the liquid 5000mL, adding the 10g particle diameter earlier is that 1mm, 10g particle diameter are that 2mm, 5g particle diameter are the activated alumina of 3mm, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the concussion of 25g atlapulgite as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 95% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.030.
Embodiment 8, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims and adds the 10g activated alumina among the liquid 5000mL earlier, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the concussion of 10g wilkinite as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 90% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.083.
Embodiment 9, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims the wilkinite that adds 25g among the liquid 5000mL earlier, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with wilkinite, adding the concussion of 25g molecular sieve as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, be purified the recovery liquid removal of impurity 81% after the processing, the acid number after the purifying treatment is 0.092.
Embodiment 10, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims and adds 25g kaolin among the liquid 5000mL earlier, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with kaolin, reclaim the concussion of liquid adding 25g gac at the styrene polymerization of separating as stated above again and handle and separate, liquid removal of impurity 82% is reclaimed in the polymerization that the solution employing gas chromatograph for determination that process is filtered is purified after the processing.Acid number after the purifying treatment is 0.098.
Embodiment 11, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims and adds the high territory of 25g among the liquid 5000mL earlier, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with kaolin, adding the concussion of 25g pure aluminium silicate as stated above in the styrene polymerization recovery liquid of separating again handles and separates, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 80% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.096.
Embodiment 12, styrene polymerization reclaim the purifying treatment method of liquid
Adding the 15g particle diameter earlier among the styrene polymerization recovery liquid 5000mL among the embodiment 1 is the activated alumina of 5mm, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adding the 5g particle diameter as stated above in the styrene polymerization recovery liquid of separating again is the activated carbon of 0.5mm, the 5g particle diameter is the aluminum oxide of 0.5mm, the 5g particle diameter is that the kaolin concussion of 0.5mm is handled and separated, reclaim at the styrene polymerization separated as stated above again that to add the 15g particle diameter in the liquid be that the atlapulgite concussion of 5mm is handled and separated, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 93% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.055.
Embodiment 13, styrene polymerization reclaim purifying treatment method---the batch process method of liquid
Select 3 grades of returnable for use, 1,2, add 5g kaolin successively in 3 grades of returnable, 5 gacs, 5 activated aluminas, the styrene polymerization recovery liquid of 5000mL embodiment 1 stirs in returnable at different levels in order or concussion stopped 1 hour, obtained the returnable that different sorbent material purifying treatment liquid join next stage more successively by vacuum filtration, liquid after the last step returnable is handled becomes final purifying treatment styrene polymerization and reclaims liquid, the solution that filters through this method adopts gas chromatograph for determination, liquid removal of impurity 83% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.085.
Embodiment 14, styrene polymerization reclaim purifying treatment method---the batch process method of liquid
Select 4 grades of returnable for use, 1,2,3, add the 10g wilkinite successively in 4 grades of returnable, the 10g atlapulgite, 10 molecular sieves, 10 pure aluminium silicate, the styrene polymerization recovery liquid of 5000mL embodiment 1 stirs in returnable at different levels in order or concussion stopped 1 hour, obtained the returnable that different sorbent material purifying treatment liquid join next stage more successively by vacuum filtration, liquid after the last step returnable is handled becomes final purifying treatment styrene polymerization and reclaims liquid, the solution that filters through this method adopts gas chromatograph for determination, liquid removal of impurity 91% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.075.
Embodiment 15, styrene polymerization reclaim the purifying treatment method of liquid---continuous online treatment method
There is the circular king-post of 2 interlayers an inside, the top interlayer is equipped with the 20g activated alumina, the bottom interlayer is equipped with the 20g wilkinite, under certain pressure (0.1MPa) and temperature (25 ℃) styrene polymerization among the embodiment 1 is reclaimed liquid 5000mL with linear velocity and 1.0 h of 0.2 m/hr
-1Space velocity adopts gas chromatograph for determination through the solution after filtering by this king-post, and being purified polymerization after the processing, to reclaim the liquid removal of impurity be 93%, and the acid number after the purifying treatment is 0.054.
Embodiment 16, styrene polymerization reclaim the purifying treatment method of liquid---continuous online treatment method
With the identical condition of embodiment 15 under, the styrene polymerization that different is among the embodiment 1 reclaims liquid 5000mL with linear velocity and the 3h of 8m/hr
-1Space velocity adopts gas chromatograph for determination through the solution after filtering by this king-post, and being purified polymerization after the processing, to reclaim the liquid removal of impurity be 87%, and the acid number after the purifying treatment is 0.067.
Comparative Examples 1, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims and adds the 50g activated alumina among the liquid 500mL earlier, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with activated alumina, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 63% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.089.
Comparative Examples 2, styrene polymerization reclaim the purifying treatment method of liquid
Styrene polymerization among the embodiment 1 reclaims among the liquid 5000mL and adds without activation treatment 50g kaolin earlier, rocked 1 hour on the earthquake machine, with vacuum filtration styrene polymerization being reclaimed liquid then separates with kaolin, adopt gas chromatograph for determination through the solution that filters, liquid removal of impurity 40% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.127.
Comparative Examples 3, styrene polymerization reclaim purifying treatment method---the batch process method of liquid
Select 4 grades of returnable for use, 1,2,3, add the 5g wilkinite successively in 4 grades of returnable, the 5g atlapulgite, 5 molecular sieves, 5 pure aluminium silicate, the styrene polymerization recovery liquid of 25000mL embodiment 1 stirs in returnable at different levels in order or concussion stopped 1 hour, obtained the returnable that different sorbent material purifying treatment liquid join next stage more successively by vacuum filtration, liquid after the last step returnable is handled becomes final purifying treatment styrene polymerization and reclaims liquid, the solution that filters through this method adopts gas chromatograph for determination, liquid removal of impurity 85% is reclaimed in the polymerization that is purified after the processing, and the acid number after the purifying treatment is 0.121.
Comparative Examples 4, styrene polymerization reclaim the purifying treatment method of liquid---continuous online treatment method
With the identical condition of embodiment 15 under, different is that styrene polymerization reclaims liquid 5000mL with linear velocity and 10 h of 4 m/hr
-1Space velocity adopts gas chromatograph for determination through the solution that filters after-filtration by this king-post, and being purified polymerization after the processing, to reclaim the liquid removal of impurity be 40%, and the acid number after the purifying treatment is 0.103.
Each embodiment different substances of table 1., particle diameter, weight ratio, batch process method and continuous online treatment method and Comparative Examples table look-up
Each embodiment different substances of table 1., particle diameter, weight ratio, batch process method and continuous online treatment method and Comparative Examples table look-up (continuing)
Claims (10)
1. a styrene polymerization reclaims the purifying treatment method of liquid, it is characterized in that, styrene polymerization is reclaimed liquid to be mixed by the certain volume weight ratio with sorbent material, adopt the method for layering adsorption filtration to handle styrene polymerization and reclaim liquid, its described sorbent material is at least a material in the atlapulgite that becomes of wilkinite, kaolin or above-mentioned substance activation treatment, aluminum oxide, activated alumina, gac, molecular sieve, the pure aluminium silicate and/or the material of multiple different-grain diameter.
2. styrene polymerization according to claim 1 reclaims the purifying treatment method of liquid, it is characterized in that described sorbent material is atlapulgite and activated alumina.
3. styrene polymerization according to claim 1 reclaims the purifying treatment method of liquid, it is characterized in that the envelope-bulk to weight ratio that styrene polymerization in the described layering adsorption filtration process reclaims liquid and sorbent material is 20 ~ 1000:1.
4. styrene polymerization according to claim 1 reclaims the purifying treatment method of liquid, it is characterized in that described layering adsorption filtration is the upper and lower two-layer big particle diameter adsorbent layer that is, the middle layer is respectively the small particle size adsorbent layer of different sorbent materials.
5. styrene polymerization according to claim 1 reclaims the purifying treatment method of liquid, and the particle diameter that it is characterized in that described sorbent material is that 0.1mm is to 5.0mm.
6. styrene polymerization according to claim 1 reclaims the purifying treatment method of liquid, it is characterized in that the method for described layering adsorption filtration, comprises batch process method and/or continuous on-line processing method.
7. styrene polymerization according to claim 6 reclaims the purifying treatment method of liquid, it is characterized in that described batch process method: the amount by styrene polymerization recovery liquid in multistage returnable adds the described sorbent material of certain proportion claim 1 respectively, styrene polymerization reclaims liquid stirring or concussion stop certain hour in returnable at different levels in order, obtain the returnable that different sorbent material purifying treatment liquid join next stage more successively by vacuum filtration, the liquid after the last step returnable is handled becomes final styrene polymerization and reclaims liquid.
8. styrene polymerization according to claim 7 reclaims the purifying treatment method of liquid, it is characterized in that the envelope-bulk to weight ratio that styrene polymerization in the described returnable at different levels reclaims liquid and sorbent material is 20 ~ 1000:1.
9. styrene polymerization according to claim 6 reclaims the purifying treatment method of liquid, it is characterized in that described continuous on-line processing method is: under certain pressure and temperature styrene polymerization is reclaimed liquid and be lower than 5 h through filtering the back by space velocity
-1Be lower than 15 m/hr with linear velocity, continuously by a king-post, the described sorbent material of claim 1 is loaded in this king-post layering successively, and the styrene polymerization that is purified after the processing reclaims liquid.
10. styrene polymerization according to claim 9 reclaims the purifying treatment method of liquid, it is characterized in that described space velocity is lower than 3 h
-1, described linear velocity is lower than 8m/hr.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103949104A (en) * | 2014-04-21 | 2014-07-30 | 江苏赛宝龙石化有限公司 | Multi-layer styrene filtering device |
| CN117384095A (en) * | 2023-12-08 | 2024-01-12 | 山东联盟磷复肥有限公司 | Decoloration method of pyrazole |
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| CN103949104A (en) * | 2014-04-21 | 2014-07-30 | 江苏赛宝龙石化有限公司 | Multi-layer styrene filtering device |
| CN117384095A (en) * | 2023-12-08 | 2024-01-12 | 山东联盟磷复肥有限公司 | Decoloration method of pyrazole |
| CN117384095B (en) * | 2023-12-08 | 2024-03-12 | 山东联盟磷复肥有限公司 | Decoloration method of pyrazole |
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