• 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:

    公开号:SU1209034A3
    申请号:SU833607934
    申请日:1983-06-23
    公开日:1986-01-30
    发明作者:Билленштайн Зигфрид；Йоахим Гольке Фритц；Хилле Мартин；Бем Роланд
    申请人:Хехст Аг (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to the composition of modified, etherified condensation of phenols to aldehydes, which is used in the method of separation of oil emulsions, in particular water-in-oil emulsions,
    The aim of the invention is to turn. the demulsifying properties of poltenjensat
    According to the invention, oxyalkylation is carried out by a limestone method used, for example, for the oxidation of alcohols, glycols and amnestomes. In this case, the sterilized phenol aldehyde condensation product can be used either as such, or as a solution in an organic solvent, preferably toluene or xylene.
    Getting oil emulsion breakers in accordance with the invention.
    Example 1. Getting semi - products CJ.
    A flask with a stirrer was charged with 94.1 g (l, 00 mol) of phenol to 3.1 g of a 50% (w / w%) solution of sodium hydroxide (1., 6% by weight of phenol, followed by at 55-60 ° C, 171 g (2.00 mol) of formaldehyde is added to it in the form (weight%) of an aqueous solution. The contents of the flask are interchangeable at 70 ° C until the content of free formaldehyde is less than 2 weight ,%. The result is a red-brownish liquid with low viscosity.
    Receiving intermediate product S and interaction - its interaction with intermediate oi,
    400 g of half-propylene glycol with an average molar mass of 1700 are dried in the presence of 2.5 g (0.6 wt.% Based on the weight of polypropylene glycol, 85% (wt.%) Potassium hydroxide for 2 hours at 110 ° C. and vacuum. created by a water jet pump. After that, 172 g of tapene is added to Heiviy at 140 ° C (43 wt.%, calculated on the weight of polypropylene glycol). After oxidation, the color of medium viscosity is obtained by oxyethylation.
    For the esterification of the component and com
    80 g (about 530 mol) of the com ponent: en; that and 486 g (0.20 mosh) of the comprescent e. the molar ratio of which is the composition of 09034 is affected by i.S:, and the pot is neutralized with a mixture of dscylbenzopsulbic acid; the content of mixture I is unrelated to the water is distilled off in a vacuum of about 2000 MPa,
    i npv; 80-85 ° C., After which, the new temperature to -40 ° C is carried out by etherification and at the same time the water formed is distilled off on Kuum. As a result, p o.p y J ayu tkrassa no-ko
    And liquid
    Oxypronilating, K 325 g of the autoclave, which is autoclave, Herodroma and phenol and formaldehyde; obtained by the described
    JS method, add 1.6 g (p, 5%) of% pa calculation of the weight of the condensation product with 85% (wt.%) Potassium hydroxide. The mixture is dried for two hours, stirring it for 2 hours at 110-120 ° C. vacuum
    20 in order of 2000 kPa and then at 120– 130 ° C and a pressure of 50–500 kPa, 107 g of propylene oxide are added over 3 hours (this corresponds to a consumption of 33 g of propylene oxide per 100 g of condensation. After the oxidation is complete, the desired product is obtained. medium viscosity fluid.
    PRI me R 2, Component and 40 get a.p: alogich: but for example 1.
    Getting component B and interacting with component 5
    500 g of polypropylene glycol with an average molar mass of 2000 is dried 3 in the presence of 1.6 g (weight% in terms of the weight of the initial / e polypropylenegty-sch-salt) 85% (wt.%) Hydrochloric acid hydroxide for 2 h at 100 ° C in a vacuum created by a water jet pump. After that, 190 g of ethylene oxide (38% by weight based on the weight of the starting polypropylene glycol) are added to it at 130-150 ° C.
    dg 1 –1 tea 1 yellowish liquid sredDLiDe.tr of the component oi com ion: in 1sub with a stirrer, g (0.40 mol) of the component is mixed with 560 g (0.20 mol) of the component,; .5 The total ratio of which is J 2: 1,: and neutralizes the mixture with phosphoric acid. The mixture is heated tar; same to: ak in the example, after which the etherification is carried out, the distillation simultaneously forms a water with
    The resulting product is diluted with 600 g of rosilolad to give B a cut of graft 3,
    those 50% xylene xylene solution (wt.%).
    Oxyalkylation.
    To 520 g of a 50% (wt.%) Xylene solution of the resulting condensation product placed in an autoclave, add 2.5 g of an 85% (wt.%) Powdered potassium hydroxide (1.0 wt.% In calculating the initial condensation product) and boiling: a mixture for 2 hours at 140 ° C, water containing xylene distilled off in it and playing the role of an azeotropic component. Then, at 125-145 C and a pressure of 50-500 kPa, a mixture of 130 g of ethylene oxide and 130 g of propylene oxide is added to the autoclave for 4 hours, which corresponds to 100 g of epoxide at a weight-ratio of ethylene oxide and propylene oxide equal to 1: 1 per 100 g of solvent free condensation product. As a result of the oxyalkylation, the desired product is obtained in the form of a 67% (wt.%) Dark solution of oxyalkylate in xylene.
    Examples 3-6. The products obtained in example 1. The amounts of the starting products are given in table 1. For comparison, it also shows the corresponding data from examples 1 and 2.
    The use of oil emulsion demulsifiers in accordance with the invention.
    1700 2000
    2000 1BOO 2500 3000
    5 th) 5 20 25
    09034Л
    Tables 2 and 2 show examples of the high efficiency of new demulsifiers when used for the separation of petroleum emulsions with a relatively high salt content in various conditions.
    Example 7. Oil from fields in northern Germany.

    -
    13.2
    A2
    50
    30 ppm active substance
    Example 8. Oil from fields in northern Germany.
    Content of sodium chloride,% Water content,% Temperature of demulsification, С Concentration of demulsifier
    Table 1
    1.5: 1 2: 1
    1.5: 1
    four:. 1: 1 3: 1
    33 g of propylene oxide 50 g of ethylene oxide and 50 g of propylene oxide 194 g of propylene oxide 400 g of propylene oxide 130 g of propylene oxide 20 g of propylene oxide
    table 2
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING ETHERIFIED PHENOLFORMALDEHYDE COMPOSITION POLYCONDENSATES For the separation of oil emulsions by the interaction of 0.5–4.0 mol of the neutralized condensation product of phenol and formaldehyde in a molar ratio of 1: 1–3 at 50–80 ° С in 1 mol of alkaline catalyst the reaction product of polypropylene glycol of a molar mass of 1300-3000 and 20-100 wt.% ethylene oxide in the presence of an alkaline catalyst 80 150 C in bulk or in an inert solvent and removing the resulting water, characterized in that then, in order to increase the demulsifying properties of the polycondensates, the condensation product is treated with 20,200 parts by weight. propylene oxide per 100 wt.h. condensation product.
    1 20'9034
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    同族专利:
    公开号 | 公开日
    EP0097897A1|1984-01-11|
    DE3367109D1|1986-11-27|
    AR246285A1|1994-07-29|
    NO832315L|1983-12-27|
    BR8303379A|1984-02-07|
    US4465817A|1984-08-14|
    EP0097897B1|1986-10-22|
    DE3223691A1|1983-12-29|
    AT23050T|1986-11-15|
    JPS5918720A|1984-01-31|
    AU1624883A|1984-01-05|
    CA1198240A|1985-12-17|
    AU555356B2|1986-09-18|
    ZA834637B|1984-03-28|
    DK293583A|1983-12-26|
    DK293583D0|1983-06-24|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2792352A|1953-02-19|1957-05-14|Petrolite Corp|Process for breaking petroleum emulsions employing oxyalkylation derivatives of certain polyepoxide modified phenol-aldehyde resins|
    NL178329C|1974-09-26|1986-03-03|Hoechst Ag|METHOD FOR PREPARING ETHERATED PHENOLALDEHYDE CONDENSATION PRODUCTS AND A METHOD FOR BREAKING CRUDE OIL EMULSIONS THEREFOR|
    US4054554A|1975-03-31|1977-10-18|Petrolite Corporation|Dehazing compositions|DE3617178A1|1986-05-22|1987-11-26|Basf Ag|POLYETHER, AVAILABLE BY REALIZATION OF ALKYLOLATED BIS-METHANES WITH POLYALKYLENE OXIDES AND THE USE THEREOF AS A PETROLEUM EMULSION SPLITTER|
    DE3809067A1|1988-03-18|1989-09-28|Hoechst Ag|METHOD FOR SEPARATING WATER-IN-OIL TYPE OF OIL EMULSIONS|
    AU643324B2|1990-10-09|1993-11-11|Bp Chemicals Limited|Phenolic resin alkoxylates|
    DE4123244A1|1991-07-13|1993-01-14|Basf Ag|METHOD FOR THE MOST EXTENSIVE RECOVERY OF ORGANIC SOLVENTS IMMiscible WITH WATER|
    DE4142579A1|1991-12-21|1993-06-24|Basf Ag|PETROLEUM EMULSION SPLITTER BASED ON AN ALKOXYLATE AND METHOD FOR PRODUCING THIS ALKOXYLATE|
    US5407585A|1993-08-16|1995-04-18|Exxon Chemical Patents Inc.|Method of demulsifying water-in-oil emulsions|
    US5609794A|1994-08-05|1997-03-11|Exxon Chemical Patents, Inc.|Demulsifier for water-in-oil emulsions, and method of use|
    DE19916946C1|1999-04-15|2000-07-27|Clariant Gmbh|Resins, useful for breaking crude oil emulsions, are prepared by condensation of a disubstituted phenol aromatic amine, benzoic acid or amide with formaldehyde followed by alkoxylation|
    US7504438B1|2001-12-20|2009-03-17|Nalco Company|Demulsifiers, their preparation and use in oil bearing formations|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19823223691|DE3223691A1|1982-06-25|1982-06-25|MODIFIED VERETHERED PHENOL-ALDEHYD CONDENSATION PRODUCTS AND THE USE THEREOF FOR THE CLEAVING OF PETROLEUM EMULSIONS|
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