CN101200507B - Method for removing solvent from chlorinated polyvinyl chloride solution - Google Patents

Method for removing solvent from chlorinated polyvinyl chloride solution Download PDF

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Publication number
CN101200507B
CN101200507B CN 200610147340 CN200610147340A CN101200507B CN 101200507 B CN101200507 B CN 101200507B CN 200610147340 CN200610147340 CN 200610147340 CN 200610147340 A CN200610147340 A CN 200610147340A CN 101200507 B CN101200507 B CN 101200507B
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China
Prior art keywords
solvent
elutriation
polyvinyl chloride
chlorobenzol
chlorinated polyvinyl
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Expired - Fee Related
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CN 200610147340
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Chinese (zh)
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CN101200507A (en
Inventor
纪利俊
朱家文
武斌
陈葵
江雄旺
胡伟敏
孙建平
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East China University of Science and Technology
Shanghai Chlor Alkali Chemical Co Ltd
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East China University of Science and Technology
Shanghai Chlor Alkali Chemical Co Ltd
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Publication of CN101200507A publication Critical patent/CN101200507A/en
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Abstract

The present invention discloses a solvent removal method which can remove solvent from CPVC chlorinated solution. According to the discipline that the solvent chlorobenzol and the water forms azeotrope in the chlorinated solution, the method adopts the method combining gas-phase spray desolventize and cross-current stripping elutriation desolventize and forms the ''gas-phase spray and cross-current stripping elutriation coupling'' desolventization process of CPVC chlorinated solution. The method overcomes the defects of the prior elutriation process, such as bad desolventization effect, high solvent unit consumption and serious environmental pollution. If the chlorobenzol desolventization process provided by the present invention is adopted, the residual chlorobenzol of resin in the exit is less than or equal to 4.6wt percents, the chlorobenzol content in the discharged hot water is less than or equal to 20ppm and the chlorobenzol concentration of the gas phase in the exit is less than or equal to 600ppm.

Description

A kind of method that from chlorinated polyvinyl chloride chloride solution, removes solvent
Technical field
The present invention relates to a kind of from macromolecular solution the technology of desolventizing, particularly a kind of method that removes solvent from chlorinated polyvinyl chloride chloride solution is used for the macromolecular material production field.
Background technology
It all is polyvinyl chloride resin to be dissolved in carry out chlorating in the solvent that solvent method is produced chlorinated polyvinyl chloride resin, used solvent is chlorobenzene or the mixed solvent be made up of the lower boiling halohydrocarbon, and the chlorated liquid that generates after the chlorination reaction need remove solvent and obtain the chlorinated polyvinyl chloride resin product.The reported technology that " removes solvent " from chlorinated polyvinyl chloride chloride solution all adopts elutriation technology, difference according to the chlorated liquid dispersing mode, elutriation technology is divided into two kinds again: a kind of is direct elutriation method, as Yao Jinyu at " produce about supervinyi chloride resin in elutriation problem inquire into " (polyvinyl chloride, 1997, (5), the Desolventizing method described in 27-31).It all is direct elutriation method that the chlorinated polyvinyl chloride chloride solution that present domestic enterprise is adopted removes solvent process, its principal character is: the solvent in the chlorated liquid is a chlorobenzene, in hot water, chlorated liquid is atomized into small droplets by two passage exterior mixing airflow atomizing nozzles, utilizes solvent and hot water formation azeotrope in the drop to remove solvent; In solvent removal, chlorinated polyvinyl chloride resin is separated out in hot water, obtains resin through solid-liquid separation.Another kind method is the emulsion elutriation method, Desolventizing method described in the German patent DE 4237148, its principal character is: the solvent in the chlorated liquid is the mixed solvent of methylene dichloride and trichloromethane, under the condition that tensio-active agent exists, by high-speed stirring chlorated liquid is disperseed to form emulsion in water, under agitation condition, emulsion is added in the hot water again, feeding water vapor in hot water is removed solvent, thereby the resin in the chlorated liquid is separated out in hot water, obtains resin through solid-liquid separation again.Report from the existing chlorinated polyvinyl chloride chloride solution technology that " removes solvent ", hot water provides solvent evaporation required most of heat in " directly elutriation method ", still to be that resin is effusive carry agent to hot water, solvent vapo(u)r that removes in the elutriation process and hot water concurrent flow, solvent and hot water can only form the one-level azeotropic vaporization, residual solvent is higher in the effusive hot water from the elutriation tower, reach more than the 170mg/L, when liquid-solid separation, solvent evaporates in a large number, both increase the solvent unit consumption, caused serious topsoil again; Difference on the chlorated liquid quality that obtains owing to every batch of chlorination reaction in " emulsion elutriation method ", cause emulsification condition to be difficult to accurate control, owing to added tensio-active agent in this method in chlorated liquid, tensio-active agent can not remove from resin when elutriation, has influenced the quality of product simultaneously.On existing literature, do not find identical with theme of the present invention or similar report as yet.
Summary of the invention
The objective of the invention is to, a kind of solvent process that removes from chlorinated polyvinyl chloride chloride solution is provided, is exactly the technology that removes the solvent chlorobenzene that proposes a kind of " gas phase spraying and the coupling of cross-flow stripping elutriation " specifically, overcomes with this to have deficiency in prior art.
Technical scheme:
Design of the present invention is as follows:
The method that removes solvent in the chlorated liquid of the present invention has been utilized spray-dired principle, removes solvent by the gas phase spraying earlier, forms the solidified chlorinated polyvinyl chloride resin; The solidified resin hot water carry down and hot water along continuous straight runs is mobile together, form cross-flow stripping elutriation with the water vapor that feeds in the hot water, cross-flow stripping elutriation process further removes the solvent in hot water and the resin, be that solvent is to remove in two processes that are connected mutually, earlier remove most of solvent in the chlorated liquid by the gas phase spraying, again in cross-flow stripping elutriation process, utilize the solvent in the further deresinate of elutriation effect, the gas phase spraying removes has only a small amount of solvent to be diffused in the hot water in the dissolving agent process, the solvent in the hot water removes by the stripping effect of water vapor.
The present invention is achieved through the following technical solutions:
A kind of method that removes solvent from chlorinated polyvinyl chloride chloride solution is characterized in that, described method is as follows:
1) chlorinated polyvinyl chloride chloride solution that will contain the solvent chlorobenzene removes solvent through the gas phase spraying, chlorobenzene concentration in the chlorated liquid is 80%~90wt%, adopt the air-blast atomization nozzle to atomize, the gas that drives atomizing is saturated or superheated vapour, the gas speed of nozzle exit is 80~200m/s, and the mass ratio of water vapor and chlorated liquid is 0.5: 1~3: 1;
2) the curing chlorinated polyvinyl chloride resin particle that forms in the atomization process is that 98~99 ℃ hot water carries down in temperature, is steam stripping agent with the water vapor, carries out cross-flow stripping elutriation further to remove solvent, and wherein, the steam stripped time of cross-flow is 20~180s.
Beneficial effect
Characteristics of the present invention are: the technology that removes the solvent chlorobenzene that has adopted " gas phase spraying and the coupling of cross-flow stripping elutriation ".The water vapor that drives the chlorated liquid atomizing both provided the required kinetic energy that atomizes, provide chlorated liquid to remove the required part heat of solvent again, the solvent chlorobenzene is to remove in two processes that mutually are connected: remove most of solvent in the chlorated liquid by the gas phase spraying earlier, form the solidified resin particle, again in the cross-flow stripping process, utilize the solvent in the further deresinate of elutriation effect, the stripping by water vapor is used for removing the solvent in the hot water.The main effect of hot water is the agent of carrying as resin, and the cured resin that forms is taken out of.Because the solvent chlorobenzene is removed in the gas phase major part, has only a small amount of chlorobenzene to enter in the hot water by diffusion, behind the cross-flow stripping, the residual chlorine benzene concentration is very low in the hot water.Therefore, technology of the present invention has reduced discharge port place solvent volatile quantity in atmosphere greatly, thereby has reduced the chlorobenzene unit consumption, has reduced environmental pollution.
Description of drawings
Fig. 1 device synoptic diagram used in the present invention
The 1-spraying gun, 2-vaporizer, 3-pipe connecting, 4-stripping chamber, 5-U type fluid-tight discharge port, 6-hot water inlet pipe, 7-steam outlet pipe, 8-shower, 9-stripped vapor pipe, the import of 10-stripped vapor, the import of 11-spray water.
Embodiment
For better understanding the present invention, the invention will be further described below by embodiment, but for embodiment do not limit protection scope of the present invention:
Embodiment 1
The chlorinated polyvinyl chloride chloride solution that contains chlorobenzene 85wt% sprays into vaporizer 2 after the airflow atomizing nozzle atomization of spraying gun 1, the speed of jet exit water vapor is 127m/s, and the mass ratio of water vapor and chlorated liquid is 2: 1, and vaporizer 2 temperature are 98 ℃.Chlorobenzene in the chlorated liquid droplet of atomizing is evaporation in a large number in the vaporizer gas phase, and it is 98~99 ℃ hot water that the cured resin particles of formation falls into vaporizer 2 bottom level mobile temperature; Hot water and its resin flow of carrying vaporizer 2 and enter stripping chamber 4, contact with the cross-flow of water stripping steam in stripping chamber 4, and the cross-flow stripping time is 30s.Through gas Chromatographic Determination, chlorobenzene content is 4.6wt% from the effusive resin of discharge port, and chlorobenzene content is 10.9mg/L in the hot water, and chlorobenzene content is 178mg/m in the gas phase of discharge port top 3

Claims (1)

1. a method that removes solvent from chlorinated polyvinyl chloride chloride solution is characterized in that, described method is as follows:
1) chlorinated polyvinyl chloride chloride solution that will contain the solvent chlorobenzene removes solvent through the gas phase spraying, chlorobenzene concentration in the chlorated liquid is 80%~90wt%, adopt the air-blast atomization nozzle to atomize, the gas that drives atomizing is saturated or superheated vapour, the gas speed of nozzle exit is 80~200m/s, and the mass ratio of water vapor and chlorated liquid is 0.5: 1~3: 1;
2) the curing chlorinated polyvinyl chloride resin particle that forms in the atomization process is that 98~99 ℃ hot water carries down in temperature, is steam stripping agent with the water vapor, carries out cross-flow stripping elutriation further to remove solvent, and wherein, the steam stripped time of cross-flow is 20~180s.
CN 200610147340 2006-12-15 2006-12-15 Method for removing solvent from chlorinated polyvinyl chloride solution Expired - Fee Related CN101200507B (en)

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CN 200610147340 CN101200507B (en) 2006-12-15 2006-12-15 Method for removing solvent from chlorinated polyvinyl chloride solution

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Application Number Priority Date Filing Date Title
CN 200610147340 CN101200507B (en) 2006-12-15 2006-12-15 Method for removing solvent from chlorinated polyvinyl chloride solution

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CN101200507B true CN101200507B (en) 2010-05-19

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CN102225963A (en) * 2011-05-13 2011-10-26 周逸明 Method for reducing acetonitrile residue in polypeptide medicament

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4049897A (en) * 1975-11-07 1977-09-20 Imperial Chemical Industries Limited Residual solvent removal from chlorinated polymers
US4358402A (en) * 1975-11-27 1982-11-09 Imperial Chemical Industries Limited Chlorinated polymers
US4381392A (en) * 1978-10-02 1983-04-26 Caffaro S.P.A. Method for removing chlorinated solvents from chlorinated polymers
DE4237148A1 (en) * 1992-11-04 1994-05-05 Bitterfeld Wolfen Chemie Thermally stable chlorinated polymers - prepd. by soln. chlorination of polymer.

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4049897A (en) * 1975-11-07 1977-09-20 Imperial Chemical Industries Limited Residual solvent removal from chlorinated polymers
US4358402A (en) * 1975-11-27 1982-11-09 Imperial Chemical Industries Limited Chlorinated polymers
US4381392A (en) * 1978-10-02 1983-04-26 Caffaro S.P.A. Method for removing chlorinated solvents from chlorinated polymers
DE4237148A1 (en) * 1992-11-04 1994-05-05 Bitterfeld Wolfen Chemie Thermally stable chlorinated polymers - prepd. by soln. chlorination of polymer.

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
姚锦余.关于过氯乙烯树脂生产中水析问题探讨.聚氯乙烯 5期.1997,(5期),27-31.
姚锦余.关于过氯乙烯树脂生产中水析问题探讨.聚氯乙烯 5期.1997,(5期),27-31. *

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