• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    1497510 Purifying a dispersion of vinyl chloride polymer HOECHST AG 4 May 1976 [16 May 1975] 18174/76 Heading C3P Monomeric matter is removed from an aqueous dispersion of a vinyl chloride polymer by a process in which: the dispersion is introduced into the upper portion of a column provided with sieve plates and contacted therein for 10 seconds up to 20 minutes and under a pressure of 600 to 1200 mm Mg with superheated steam at 100‹ to 150‹ C flowing countercurrently with respect to the dispersion; the polymer dispersion so treated is removed from the column base portion; and a vaporous matter mixture issuing at the head of the column is condensed stagewise so as to recover an aqueous phase and the monomeric matter.
    公开号:SU841591A3
    申请号:SU762351858
    申请日:1976-04-29
    公开日:1981-06-23
    发明作者:Охородник Александер；Кайзер Карл；Вессельманн Рудольф
    申请人:Хехст Аг (Фирма)；
    IPC主号:
    专利说明:

    54) METHOD FOR CLEANING (SYO) VINYL CHLORIDE POLYMERS FROM (CO) MONOMERS The goal is achieved by the fact that the dispersion of (co) polymer with a content of Using a solid, 10-60 wt.% is introduced into the upper part of the column, equipped with sieve plates, and treated in countercurrent with water vapor with a pressure of 600-1200 mm Hg. at 100 for 0.5–20 min followed by a tap — a (co) polymer dispersion from the bottom of the column. In addition, it is advantageous to preheat the (co) polymer dispersion prior to entry into the column to 6090 ° C. In contact with rising steam in the column, heated predominantly to lOO-llO c, the temperature in the upper part of the column is 90-100 C. The pressure in the column is preferably 7001100 mm Hg. The amount of water vapor exiting through the top of the column is relatively small and amounts to 1-5% by weight of water based on the amount of dispersion required. The total exposure of the polymer dispersion in the column is 0.310 minutes. A distinctive feature of the method is that with stepwise condensation of the vapor mixture withdrawn through the "upper part of the column, the precipitated water phase is combined with (polymer dispersion before degassing monomers. In order to extract monomeric vinyl chloride from WATER polyvinyl chloride dispersions, the following properties of vinyl chloride read-water-polyvinyl chloride and their trace should be taken into account. The solubility coefficient ot of vinyl chloride in water according to Bunsen, at temperature of NO. 0, and SO has the following spruce: at 0, 2 volumes of vinyl chloride / volume of water 20 1 0.5 60 0.1 O - Solubility coefficient oL of vinyl chloride in a Bunsen water dispersion of polyvini chloride. The latter, with a solids content, dis-7 Persia amounts to 33 weight %: at 5 volumes of winch chloride / volume of water 18 3 2 1 0,6 Solubility of vinyl chloride in polyvinyl chloride, for example in a polyvinyl chloride with an average particle size between 60-120 µm and K 70 depending on temperature, the following amounts of vinyl chloride dissolve: { ei about 1100 g of vinyl chloride / 1 kg - polyvinyl chloride, 24 50 40 24 60 10 4 Co. ffitsient vinillorida distribution between water and about polivinilhloidom Ijl5. With a very efficient mass exchange, the individual phase of the mixtures establish phase equilibria in the temperature range between 90 and 10 to 100 s. The temperature range above a deterioration in the quality of the product of polyvinyl chloride, and the deterioration of the quality of the product can be prevented if the temperature effect on polyvinyl chloride is limited in time to a few minutes. In addition, the successful removal of monomers from aqueous dispersions of polyvinyl chloride in the temperature range between 90 and is ensured only when phase equilibrium is established through effective mass exchange and there is a corresponding gas phase for the transportation of onomers. The drawing shows the device, the implementation of the proposed method. For the purpose of heating the stripping column 2, steam 1 is first introduced in steam until condensate is obtained in heat exchanger 3. The stripping column 2 consists of a perpendicularly arranged column in which the sieve plates 4 are horizontally disposed at certain distances. The sieve plates 4 differ from the internal devices of conventional columns with sieve plates in that they do not have a special inflow and drain of the liquid. The diameter of the gas or liquid through holes 5 in the sieve plates is from 1 to 10 mm, and the total surface of the through holes is from 5 to 50% of the column cross-section plane. After heating of the Stripping column 2 from the collector 6, the pipeline 7 through the upper part of the Stripping column 2 supplies the amount of (co) polymer dispersion with an average particle size of 20-500 microns, preheated in the heat exchanger 8 and measured in the dosing unit 9. The steam supply through line 1 is controlled so that the temperature in the upper part of the stripping column 2 is 90-100 ° C, and the amount of steam is enough to distill the monomer from the (co) polymer dispersion. The dispersion without monomer is removed in the lower part of the stripper column 2 through conduit 10, in which case it transfers its heat in heat exchanger 8 to pre-heat the fresh polymer dispersion. The holding time of the (co) polymer dispersion in the sponge colo 2 is determined mainly by the number of sieve plates It ranges from 5 to 50, as well as the quality of particles of solid dispersion materials. The steam entering the column serves, along with partial heating of Persia to the required temperature, mainly for distilling and rejecting the monomer from the dispersion. water vapor and monomer leaving through the upper part of the stripping column 2 and through pipe 1 is cooled in the heat exchanger 3 to a temperature of from 5 to 20 ° C, so that the water vapor condenses. The condenser, which, according to the monomer solubility in water, contains a certain amount of dissolved monomer, can be discharged through pipe 13 and connected to fco) polymeric dispersion of collector 6. Non-condensable monomer in heat exchanger 3 is led through pipe 41 to reservoir 12 and also through conduit 14 to heat exchanger 15 and condensed by cooling to 15 ° C. The liquefied monomer is collected in reservoir 16, from where it is in gaseous or liquid state through pipelines 17 or 18 can be received for further use. The proposed method is technically progressive, since it is more effective and, in addition, more environmentally friendly and less susceptible to damage, in contrast to conventional methods for removing monomer from polymers. For example, polymers purified by the proposed method contain only traces of monomers of the order of 10 ppm so that for polymers, because of their high degree of purity, new application possibilities are revealed that have not yet been known due to the lack of internal cleaning degree polymers containing relatively high amounts of monomer. The implementation of the method in a stripping column equipped with such screen plates eliminates the possibility of contamination and the formation of deposits in the through holes of the screen plates. It is mainly suitable for removing monomers from such aqueous tco) polymer dispersions, in which polymer particles are heavier than water. Example 1. According to the technological scheme shown in the drawing, the polyvinyl chloride dispersion is purified from vinyl chloride, the dispersion contains 6jOOO ppm. vinyl chloride, the presence of a solid polymer complies with 35 wt.%, while polyvinyl chloride has a value of K equal to 70, an average particle size of 65 µm and a consumption of softener is 27.7%. The internal diameter of the stripping column 2 used to purify the dispersion is 100 mm, and the column itself has 20 screen plates. The sieve plates are located in the column at a distance of 150 mm and have 250 through holes with a diameter of 2.5 mm. According to the pipe of the pipe 1 to the steam column 2, water vapor with a temperature and pressure of 760 mm Hg. it enters until condensable water is formed in the heat exchanger 3 cent. Upon further steam supply, the aqueous polymer dispersion enters the upper part of the stripping column 2 at a flow rate of 48 l / h, respectively, with an average duration of keeping the dispersion for 1 minute. Steam supply to the column is adjusted so that about 3% by weight of condensate forms in terms of the number of dispersions loaded per hour, the temperature in the upper part of the column is 95-100 ° C and the temperature in the lower part of the column is 102105 ° C. The pressure difference in the column is 50-80 mm Hg. t. In the tank 12, 1.5 liters of water containing vinyl are collected per hour, which is then combined with the polymer dispersion to be cleaned. The dispersion at the bottom of the stripping column 2 contains less than 1 ppm in the aqueous phase and less than 10 ppm in the polyvinyl chloride. vinyl chloride. The residual content of vinyl chloride in the polymer dispersion is determined by gas chromatography. In the heat exchanger 5, 125 g of vinyl chloride per hour is condensed at a temperature. Example 2. The procedure is the same as in Example 1, in which case the polymer dispersion is cleaned containing solid polyvinyl chloride with a value of K 62. The average size of the polymer particles is 120 µm and the consumption of the softener is 13.5%. Dispersion contains 5200 parts per million of vinyl chloride. The dispersion passing rate in the column is 48 l / h, respectively, according to the average duration of keeping the evaporation for 2 minutes. The steam supply to the column is adjusted in such a way that about 5 weight is formed in heat exchanger 3. % of condensate based on the amount of dispersion loaded hour. The purified dispersion contains another 10 ppm of vinyl chloride in solid material and less than 1 ppm. Vinyl chloride in water. Example 3-7. Used in the reamer 1 column is equipped with such a braz so that it can work as
    with reduced pressure and with increased. The polymer dispersion to be purified corresponds to that in Example 1. 0 1 The search for dispersion is carried out under the conditions given in the table.
    Purification under these conditions JQ isomerized polymers contain about 1 ppm of water in the aqueous solution. vinyl chloride. Polyvinyl chloride contains about 10 ppm. vinyl chloride.
    Example 8. A water dispersion of a copolymer consisting of 90% by weight of vinyl chloride and 10% by weight of% vinyl acetate with a treatment rate of 40 l / h is introduced into a column with sieve plates. The polymer dispersion introduced contains 4000 ppm. vinyl chloride. Through the supply of water vapor in the upper part of the column, the temperature is kept at 95-99 ° C and in the lower part of the column - 102-104 ° C at a pressure of 760 mm Hg. The purified dispersion contains another 45 10 ppm. vinyl chloride in the copolymer and less than 1 ppm. in water.
    Example 9. The operation is performed in accordance with Example 1, in which case in one case the dispersion of polymer Persia before entry into the column is preheated in the heat exchanger 8, and in the other case is not heated. The results of both experiments show that with pre-heating the dispersion, the amount of water vapor supplied through pipeline 1 is 40% less than with the method without pre-heating the dispersion.
    Thus, when implementing the proposed method, a very effective purification of (co) polioch (co) monomegmers of vinyl chloride occurs, which expands the scope of their application.
    权利要求:
    Claims (2)
    [1]
    1. A method for purifying (co) polymers of vinyl chloride from (co) monomers by treating (co) polymers with steam during heating, characterized in that, in order to increase the cleaning efficiency, dispersion of (co) polymer with a solids content of 10-60 weight ,% is introduced into the upper part of the column, equipped with sieve plates, and treated in countercurrent with steam with a pressure of 600-1200 mmHg. at 100-150 ° C for 0.5-20 minutes, followed by removal of the (co) polymer dispersion from the bottom of the column.
    [2]
    2. The method according to claim. 1, that is, with the fact that the (co) polymer dispersion is heated to 60-90 ° C before entering the column.
    Sources of information taken into account in the examination
    1. The patent of Germany No. 1248943,
    cl. 39 b, 1/88, published. 1967.
    2.Patent of France No. 2193042,
    cl. From 08 f 1/96, published 1974 (prototype).
    - / (
    类似技术:
    公开号 | 公开日 | 专利标题
    SU841591A3|1981-06-23|Method of purifying /co/polymers of vinyl chloride from /co/monomers
    US3165452A|1965-01-12|Submerged combustion and flash evaporation system and process
    US4260461A|1981-04-07|Vapor compression distillation apparatus and method
    CN107188199A|2017-09-22|It is a kind of that ammonium sulfate, the Processes and apparatus of sodium sulphate are reclaimed from waste water
    SU1378781A3|1988-02-28|Method of separating carbamide,ammonia and carbon dioxide from diluted water solutions
    JP2520317B2|1996-07-31|Ultrapure water production apparatus and method
    US2336493A|1943-12-14|Distillation of organic liquids polymerizable by heat
    US3926591A|1975-12-16|Regeneration of scrubbing agent used for the removal of co' 2 'and h' 2's from gases containing polymerizable hydrocarbons
    US4171427A|1979-10-16|Process for continuously removing monomers from an aqueous dispersion of a polymer
    US4261818A|1981-04-14|Method for making separations from aqueous solutions
    JP4674681B2|2011-04-20|Method and apparatus for treating water for evaporation
    US2471893A|1949-05-31|Treatment of citrus waste press water
    US3234125A|1966-02-08|Removal of water from aqueous solutions
    GB1397002A|1975-06-11|Process and apparatus for making fresh water by freezing brine
    US2593862A|1952-04-22|Method for polymerization of formaldehyde and recovery of paraformaldehyde
    US3790448A|1974-02-05|Method of purifying waste fluid
    CN109796366A|2019-05-24|A kind of high concentration DMF or DMAC rectifying and purifying system and method
    US2056748A|1936-10-06|Process for phenol recovery
    JP3162525B2|2001-05-08|Continuous treatment method for removing residual monomer from aqueous latex of synthetic polymer and apparatus for performing the same
    CN104724776B|2018-04-03|Devices and methods therefor in pressure evaporating indirect steam incorporation press water
    GB1076520A|1967-07-19|Improvements in apparatus for use in evaporative processes
    US3095295A|1963-06-25|Chemical process
    JP2005105047A5|2006-09-07|
    JPH0815529B2|1996-02-21|Vapor regeneration method for solvent recovery equipment
    SU481296A1|1975-08-25|The method of cleaning gases from acidic components
    同族专利:
    公开号 | 公开日
    FR2311037B1|1981-12-31|
    DD124253A5|1977-02-09|
    NL160841B|1979-07-16|
    ES447280A1|1977-06-16|
    SE7602710L|1976-11-17|
    BE841838A|1976-11-16|
    IE43107B1|1980-12-17|
    GB1497510A|1978-01-12|
    LU74948A1|1977-02-14|
    NO761676L|1976-11-17|
    HU174924B|1980-04-28|
    JPS51140985A|1976-12-04|
    AT352393B|1979-09-10|
    DE2521780C2|1982-10-21|
    CH601358A5|1978-07-14|
    CA1278638C|1991-01-02|
    FR2311037A1|1976-12-10|
    PL103008B1|1979-05-31|
    DK213576A|1976-11-17|
    ATA354776A|1979-02-15|
    IE43107L|1976-11-16|
    JPS5246994B2|1977-11-29|
    NL7605200A|1976-11-18|
    IT1061284B|1983-02-28|
    NO146284B|1982-05-24|
    CS191306B2|1979-06-29|
    YU121376A|1982-02-28|
    DE2521780A1|1976-11-18|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    NL129660C|1964-08-24|
    US3816379A|1971-07-26|1974-06-11|Exxon Research Engineering Co|Monomer and solvent recovery in polymerization processes|
    BE793505A|1972-12-29|1973-06-29|Solvay|Process for removing residual vinyl chloride present in the polymer|
    NO752264L|1974-08-29|1976-03-02|Huels Chemische Werke Ag|
    DE2450464A1|1974-10-24|1976-04-29|Basf Ag|PROCESS FOR LOW EMISSIONS REMOVAL OF VINYL CHLORIDE FROM POLYMERIZES OF VINYL CHLORIDE|
    DE2509937C3|1975-03-07|1981-04-16|Hoechst Ag, 6000 Frankfurt|Device for the aftertreatment of homo- and copolymers of vinyl chloride|
    DE2520591C3|1975-05-09|1980-11-06|Hoechst Ag, 6000 Frankfurt|Process and device for the continuous treatment of aqueous homo- and copolymer dispersions, the polymer content of which is at least 50% by weight polymerized|JPS5298591U|1976-01-20|1977-07-25|
    NZ184661A|1976-07-27|1979-08-31|Ici Australia Ltd|Removing monomer from vinyl chloride polymers|
    DE2640546C2|1976-09-09|1982-07-01|Hoechst Ag, 6000 Frankfurt|Process for the continuous removal of vinyl chloride from an aqueous dispersion of homo- and copolymers of vinyl chloride|
    DE2640592C2|1976-09-09|1989-03-02|Hoechst Ag, 6230 Frankfurt, De|
    DE2800608A1|1977-04-11|1978-10-19|Buna Chem Werke Veb|PROCESS FOR THE DEMONOMERIZATION OF POLYMER DISPERSIONS, PREFERABLY POLYVINYL CHLORIDE DISPERSIONS|
    DE2718858C2|1977-04-28|1991-10-24|Hoechst Ag, 6230 Frankfurt, De|
    DE2718857C2|1977-04-28|1992-07-30|Hoechst Ag, 6230 Frankfurt, De|
    JPS6111241B2|1977-06-21|1986-04-02|Chisso Corp|
    DE2744462C2|1977-10-03|1982-09-16|Wacker-Chemie GmbH, 8000 München|Process for preventing foam formation during the removal of residual monomers from aqueous polymer dispersions|
    US4201628A|1977-10-07|1980-05-06|The Goodyear Tire & Rubber Company|Separation apparatus|
    DE2746909C3|1977-10-19|1982-03-11|Hoechst Ag, 6000 Frankfurt|Process for the continuous removal of residual hydrocarbons from polyolefins|
    US4200734A|1977-11-21|1980-04-29|Diamond Shamrock Corporation|Process for polymerization of polyvinyl chloride and VCM monomer removal|
    DE2759097C2|1977-12-30|1987-03-05|Norsk Hydro A.S., Oslo, No|
    US4228273A|1978-09-05|1980-10-14|Tenneco Chemicals, Inc.|Process for the removal of vinyl chloride from aqueous dispersions of vinyl chloride resins|
    DE2855146C2|1978-12-20|1983-04-28|Chisso Corp., Osaka|Process for removing residual monomeric vinyl chloride from an aqueous dispersion of a polyvinyl chloride resin powder|
    DE2903586A1|1979-01-31|1980-08-14|Hoechst Ag|METHOD FOR THE CONTINUOUS REMOVAL OF RESIDUAL HYDROCARBONS FROM POLYOLEFINS AND DEVICE FOR CARRYING OUT THE METHOD|
    US4402916A|1981-06-30|1983-09-06|Marathon Oil Company|Dilution apparatus and method|
    JPH0444884B2|1987-06-19|1992-07-23|Chisso Corp|
    WO1996018659A1|1994-12-12|1996-06-20|C.I.R.S. S.P.A.|Method and plant for the production of polyvinylchloride in aqueous suspension with recovery of refluxes|
    JP3950743B2|2002-06-03|2007-08-01|キヤノン株式会社|Method for producing toner particles|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2521780A|DE2521780C2|1975-05-16|1975-05-16|Process for the continuous removal of monomers from an aqueous dispersion of a polymer|
    [返回顶部]