• 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:SU1225492A3
    申请号:SU823506054
    申请日:1982-10-27
    公开日:1986-04-15
    发明作者:Билленштайн Зигфрид；Фройндль Хильдегард；Виммер Игнац；Йоахим Гольке Фритц；Маценка Йоханнес
    申请人:Хехст,Аг (Фирма)；
    IPC主号:
    专利说明:

    f
    The invention relates to the exfoliation of water-in-oil emulsions,
    The aim of the invention is to increase the delamination depth.
    This goal is achieved by using a new efficient demulsifier, which uses the product of the interaction of propylene oxide block copolymer and ethylene oxide with an average mol.m. 1900-3800, containing 10-30 wt.% Of ethylene oxide and 70-90 wt.% Of propylene oxide, obtained by adding ethylene oxide to the polypropylene glycol in the presence of an alkaline catalyst (component a), oxyethylated or ethoxylated and hydroxypropylated alkylphenolformaldehyde resin, obtained by the interaction of para- and / or ortho-x-phenol with carbon atoms in the alkyl group with formaldehyde, taken in a molar ratio of 1S: (1-1.3), in the presence of an acid catalyst at 100-160 ° C, followed by oxidation or ethoxylation and propoxylation in the presence of an alkaline catalyst at 100-160 C 2-32.6 moles of epoxyde per phenolic hydroxyl group (component b), as well as formaldehyde at a mass ratio of components a to b equal to (9.8 - 40): 1, and the amount of formaldehyde, 0.8-1.3 times stoichiometric, based on the total number of hydroxyl groups and b when carrying out the process of interaction in the presence of an acid catalyst at 100-160 С (component c) . The demulsifier is added to the emulsion 10-100 mas. on 1 million may, h. emulsion.
    Example 1. The product of block polymerization (component a),
    Polypropylene glycol having an average mol.m. 2000, is subjected to an exchange reaction in a known manner in the presence of an alkaline catalyst with such a large amount of ethylene oxide to obtain an adduct with an ethylene oxide content of 20 wt.% In the final product (hydroxyl number 46)
    Alkylphenol-aldehyde resin (component b).
    It is obtained by condensation at 115-160 ° C in the presence of a catalytic
    254922
    the amount of dodecyl benzole sulphonic acid I - nonylphenol with an equivalent amount of formal solution (35% by weight), freed the reaction mixture from water by distillation with xylene and neutralized.
    Then, after adding a catalytic amount of lye, the obtained resin is reacted with
    to 120-160 C with such amount of ethylene oxide to 1 eq. resin; i.e. per one hydroxyl group in the composition of phenol, accounted for 5 mol of ethylene oxide. 20% by weight
    The 15 xylene solution has a hydroxyl number of 24. This solution is component b.
    The product corresponding to the de-waste product according to the invention.
    20 280 g of component a 79 g of component b (which corresponds to the mass
    the ratio of a to b in terms of 100% components 181) and 280 g di-H - butylfor small is placed in a flask „
    skabzhennuyu stirrer and nozzle for the distillation of water, together with g of a 35% by weight aqueous solution of formalin (which contains 11, g of formaldehyde is a component in that
    corresponds to its stoichiometric amount, calculated on the hydroxyl groups containing in components a and b). While stirring, 2.4 g of concentrated sulfuric acid (corresponding to 0.6 wt.% Sulfuric acid, based on the mass amount) are added and the reaction temperature is slowly raised to 160 ° C while distilling water. After approximately 6 hours, the reaction is cooled to approximately 50 seconds and the di-n-butylformal is distilled off in a vacuum created by a water-jet pump (about 2000 Pa), and the temperature in the lower part is again increased to 160 C. After cooling to 100 ° C, 10 g is neutralized. 30% sodium methoxide solution. A brown, viscous, soluble product is obtained.
    in organic solvents (e.g., xylene).
    Example 2. 540 g of the component of example 1 and 30 g of p -nonylphenol-formaldehyde resin, ethoxylated with ethylene oxide, in an amount of 5 mol, similar to component b in example 1 in the form of a 90% w / w solution in xylene having gid3
    The roxyl number 107 (mass ratio of a to b is 20: 1) is mixed with 20 g of a .35% aqueous solution of formalin (20 g corresponds to 1.1 times the amount of formaldehyde relative to the hydroxyl groups present in a and b After adding 3.3 g of concentrated sulfuric acid (which corresponds to 0.6 wt.% Sulfuric acid relatively), I mix
    3 hours at 100 ° C, then heated to 140 ° C and, upon reaching this temperature, a vacuum is created by means of a water jet pump. After a 6-hour period of condensation at 140 ° C, it is cooled and neutralized with a solution of sodium methylate, as indicated in the example. A brown, viscous product is obtained that is soluble in organic solutions.
    Example 3. 150 g of the component a in example 1 and 8.5 mach. ti-nilphenol-formaldehyde resin, ethoxylated ethylene oxide in a quantity of 5 mol (by weight in xylene, hydroxyl number 107) in example 2 as component b, is stirred in a flask equipped with a stirrer, together with 2.5 g of paraformaldehyde, which corresponds to 1.1 times the stoichiometric amount of formaldehyde (component c) in relation to the hydroxyl groups in a and b, the mass ratio of a to b is 19.6: 1. After adding 0.88 g (0.55 wt.%) by concentrating sulfuric acid, the reaction mixture is slowly heated with stirring SRI to 140 C and additionally stirred for 1 hour at this temperature. They create a vacuum with a water-jet pump and press
    4 h at 140 C. After this period of condensation, the mixture is cooled and neutralized with sodium methoxide solution, as indicated in Example 1. A dark brown, viscous product is obtained which is soluble in organic solvents.
    Example4. 150 g of component a according to example 1 and 1.7 g and -nonylphenol formaldehyde ethoxylated with ethylene oxide in an amount of 5 mol (90% by weight in xylene, hydroxyl number 107) in example 2 as component b (corresponds to the mass ratio a to b based on 100% components



    9.8: 1), are mixed in a flask equipped with a stirrer, together with 7.2 g of a 35% w / w aqueous solution of formalin (corresponding to a 1.1-fold stoichiometric amount of formaldehyde relative to hydroxyl groups a and b). After adding 0.8 g (0.6% by weight) of concentrated sulfuric acid, it is stirred for 2 hours at 100 ° C, then heated to 140 ° C and held at this temperature for 1.5 hours. A vacuum is created with a water-jet pump and heated for another 6 hours at 140 C. After cooling and neutralization with sodium methoxide solution, a dark brown viscous product is obtained, soluble in organic solvents.
    PRI me R 5. 250 g of component a in example 1 and 9.8 gp-tert-butylphenol-formaldehyde h | p5 | req, obtained by condensation of n-tert-butylphenol and formaldehyde analogously to the resin of example 1, but at a temperature - re 100-145 C followed by ethoxylation at 130-160 C with ethylene oxide in an amount of 2 mol, similar to preparation of component b in example 1, as component b (in the form of a 65% w / w solution in xylene) a ratio of a to b equal to 40: 1, mixed together in a flask equipped with a stirrer, with 10.8 g of a 35% by weight aqueous solution of formalin (10 , 8 g corresponds to a 1.1-fold stoichiometric amount of formaldehyde, calculated on the hydroxyl groups present in). With stirring, 1.5 g (0.6% by weight of concentrated sulfuric acid) is added dropwise, then after 2 hours of stirring the mixture at 100 ° C, it is kept at 140 ° C for 1 hour. After creating a vacuum with a water jet pump, the reaction mixture is stirred 3 hours at 140 ° C, after cooling, neutralized with sodium methoxide solution. The reaction product is a reddish-brown, viscous mass, soluble in organic solvents.
    Example 6.150 g of component a according to Example 1 and 8.4 g of a nonylphenol-formaldehyde resin obtained from p-nonylphenol and formaldehyde by condensation at 100-145 ° C, as in Example 1, which is reacted
    with 22.6 mol of propylene oxide, then with 10 mol of ethylene oxide, as in example 1, but at 100-160 ° C (96% in xylene, hydroxyl number 53.8) as component b (corresponds to the mass ratio a cb, calculated on 100% components 18.6: 1), is mixed with 6.2 g of a 35% w / w aqueous solution of formalin in a flask equipped with a stirrer (6.2 g correspond to 1.1 -fold stoichiometric amount of formaldehyde relative to hydroxyl groups (y). After adding 0.8 g (0.5 wt.%) Of concentrated sulfuric acid, the condensation is carried out for 2 hours at, then at 140 ° C. After that, a vacuum is created by means of a water-jet pump and additionally kept for 10 hours at. Following neutralization with sodium methylate solution, a dark viscous product is obtained that is soluble in opium.
    solvent solvents
    Example. Polypropylene glycol with an average mol. m. 1700 is subjected to an exchange reaction in a known manner in the presence of an alkaline catalyst with such a large amount of ethylene oxide to obtain an adduct with an ethylene oxide content of 27 wt.% in the target product. This product is a component of a. 230 g of i-nonylphenol is reacted in the presence of a catalytic amount of sodium hydroxide with 43 g of 91% by weight para-formaldehyde (which is an amount 1.3 times the stoichiometric) at 120-160 ° C. Paraformaldehyde is added in separate portions. To the end, the water formed during the reaction is removed by distillation with xylene, and is heated to a temperature not higher than 160 ° C.
    The obtained resin without additional alkalization is subjected to reaction in a known manner at 00-160 ° C with such large quantities of ethylene oxide and propylene oxide, so that 6.7 mol of ethylene oxide and 6.0 mol of propylene oxide can be obtained in succession for the reaction. phenolic hydroxyl group. I get a 90% xylene solution of a block polymer formed of resin and ethylene oxide (oxide
    5 C 5 Ci
    five
    0 5 0 5
    0 5
    propylene) has a hydroxyl 4Hv ratio of 66.4 and is component b. Next, 150 g of component a and 8.5 g of component b (which corresponds to a mass ratio of 100% components a to b 20: 1) are mixed with 6.5 g of a 35% by weight aqueous solution of formalin (6.5 g correspond to 1.07 times the stoichiometric amount, based on the available hydroxyl groups). After adding 0.9 g (0.6 wt.%) Of the concentrated sulfuric acid, the mixture is stirred at 100 ° C for 2 hours, then heated to 140 ° C and a vacuum pump is created. After condensation for 6 hours at 140 ° C in vacuum the mixture is cooled and neutralized with sodium ethyl acetate solution. The resulting product is a brown viscous xylene liquid soluble.
    Try on 8-10. Compounds similar to those described above are obtained. In tab. I presents the characteristics of components a and b and the conditions for preparing the compounds.
    The following examples illustrate the degradation of oil water-in-oil emulsions by adding the products prepared in examples 1-10 as a demulsifier.
    PRI me R 11. Syrah oil from the Alpine region.
    Moisture content 50.50 wt.%.
    Salinity of 0.49 wt.%.
    Demulsification temperature 50 C.
    The results are presented in table 2.
    Example 12. Emulsion of crude oil from a field in the region of southern Germany.
    Moisture content is 51.50 wt.%.
    The salinity of 0.76 wt.%.
    Demulsification temperature 50 C.
    The results are presented in table. 3
    Example 13. A crude oil emulsion, representing crude oil from the Pre-Alpine region, was treated with a moisture content of 50 and a salinity of 0.25 wt.%.
    The results are presented in table. four.
    Example 14, Emulsion of crude oil from Saudi Arabia,
    Moisture content 17.5 May.%.
    Salinity of 12.2 wt.%.
    Demulsification temperature 70 C.
    The results are given in table. five. "
    Example 15, crude oil emulsion from the USSR, Raevsk type.
    Moisture content 66 wt.%.
    Salinity of 18 wt.%.
    Demulsification temperature 40 C.
    The results are given in table. 6
    Example 16: A crude oil emulsion, representing crude oil from the Pre-Alpine region.
    Moisture content 50 wt.%.
    The salinity of 0.50 wt.%.
    Demulsification temperature 50 C.
    The results are given in table. 7
    Example 17. Worked on emul
    this crude oil from the Voralpen region.
    Block copolymer (component a): average mol, m
    Ethylene oxide, wt.%
    about
    Oxyalkylated alkylphenol formaldehyde resin (component b): alkyl group nol
    The amount of formaldehyde per 1 mol of alkylphenol, mol
    Alkylphenol condensation temperature
    and formaldehyde in the presence of acid
    catalyst, with
    The amount of epoxide on phenolic hydro-20 oxide 2 oxide 2 oxide
    xyl group, mole
    Oxyalkylation temperature, C
    b and c
    mass ratio of a to b
    Condensation product a, b and c
     „
    The amount of formaldehyde from stoichiometry 1.0
    Q
    Interaction temperature, C100-16
    Moisture content 50 wt.%,
    The salinity of 0.82 wt.%.
    Exfoliation temperature 30 C.
    The results are given in table. eight.
    Example 18. Processed emulsion of oil from Niederzahsen.
    The moisture content of 44 wt.%.
    Salinity 9.7 wt.%.
    Exfoliation temperature 30 ° C,
    The results are given in table. 9.
    Example 19. A crude oil emulsion was processed from the Vorpan area with a water content of 50 wt.% And a salt of 0.5 wt.%.
    Exfoliation temperature.
    The delamination results are shown in Table. ten.
    Table 1
    3800 15
    3200 30
    1900 10
    (1-NONSh1 o- and P -Do-tert-butyl decyl
    one
    t
    1,3
    100-145 100-160
    100-145
    ethylene ethylene ethylene
    10 propylene oxide
    130-160 100-160
    130-160
    10: 1
    To}) demulsifier based on resin 50 US patent No. 2499368 (2) in example 1 50
    32 76
    78 78 80 85
    40 98 100 100 100 100



    de- and 30 C


    50 50
    30 30
    20
    four
    O 1 o
    Table l
    78 78 80 85
    0.6
    0.1
    ABOUT
    ABOUT
    36 3840
    94 9496
    013
    18 2022
    34 80 96
    18.2 0.3
    thirty . 0.5
    ABOUT
    Oh oh
    6276 78 80
    3680 90 96
    O000
    2260 62 64
    2056 84 92
    1.6
    0.4
    12.8 0.6
    ABOUT
    Oh oh
    about
    (1) Demulsifier on the basis of syule, provided with cross-linked molecular structures, according to the Federal Republic of Germany patent
    No. 1642825
    (2) Sewing de-emulsifier according to the German patent
    No. 2445873
    (3) For example 2
    Table3
    52
    64 68 82 88 2.8
    Temperature demulsification
    (1) A mixture of 150% by weight block copolymer a and 8.5 parts by weight hydroxyethyl resin according to example 3, mine processing forms | L5Inom
    (2) In example 3 Test experience
    Temperature dee fyll gavani
    25 ° С
    1010
    0112 .10 16 22 30 44
    8 40 68 76 80 86 88 88 90 000 00000 О
    (1) De-emulsifier based on resin provided (cross-linking of molecular structures, according to the p-atenta of HGF
    No. 1642825
    (2) Crosslinked de-emulsifier according to the German patent
     2445873
    T a b l and c a 4
    Table5
    ten
    18
    34 36 36
    thirty
    52
    68
    74 80
    4.0
    based on resin, provided with cross-linked molecular structures, by the Patented Polymer, obtained by block copolymerization by
    Table
    Table
    (1) Crosslinked de-emulsifier according to the German patent
    (1) Sewing de-emulsifier according to the German patent
    No. 2445873 50
    (2) For example 9 50
    (3) Control
    experience (1) 15
    (2) 15 (3)
    010 24 34 70 72 10.0
    110 44 78 90 94 0.5
    Table
    Table9
    Compiled by N. Kirillov Editor M. Tsitkina Techred M. Morgeital Proofreader G. Reshetnik
    Order 1972/63 Circulation 482Signature
    VNIIPI USSR State Committee
    for inventions and discoveries 11E035, Moscow, Zh-35, Raushsk nab., 4/5
    Production and printing company, Uzhgorod, Projecto st., 4
    Table 10
    权利要求:
    Claims (1)
    [1]
    METHOD FOR LAYERING OIL EMULSIONS TYPE WATER IN OIL by adding 10-100 parts by weight per 1 million parts by weight demulsifier emulsions, in that, in order to increase the delamination depth, a product obtained by reacting a block copolymer of propylene oxide and ethylene oxide with an average molecular weight of m is used as a demulsifier. 1900-3800, containing 10-30 wt.% Ethylene oxide and 70-90 wt.% Propylene oxide obtained by attaching to ethylene oxide polypropylene glycol in the presence of an alkaline catalyst (component a), ethoxylated or ethoxylated and oxypropylated alkylphenol formaldehyde resin obtained by the interaction of para- and / or orthoalkylphenol with 412 carbon atoms in the alkyl group with formaldehyde, · taken in a molar ratio of 1: (1-1.3), in the presence of an acid catalyst at 100-160 ° С followed by ethoxylation or ethoxylation, etc. by oxylation in the presence of an alkaline catalyst at 100-160 ° C with 2-32.6 moles of epoxide per phenolic hydroxyl group (component b), as well as formaldehyde with a mass ratio of components a to b equal to (9.8-40): 1, and the amount of formaldehyde, 0.8-1.3 times stoichiometric, based on the total number of hydroxyl groups a and b during the interaction process in the presence of an acid catalyst at 100-160 C (component c).
    . SU 1225492
    1225492 2 quantities of dodecylbenzenesulfonic acid N-nonylphenol with an equivalent amount of formaldehyde solution (35 wt.%), The reaction mixture is freed from water by distillation with xylene and neutralized.
    Then, after adding a catalytic amount of alkali, the resulting resin is reacted at 120-160 ° C with such an amount of ethylene oxide to 1 equivalent. resins i.e. for one hydroxyl group in the composition of phenol, 5 mol of ethylene oxide accounted for. 20% by weight
    The 15 xylene solution has a hydroxyl number of 24. This solution represents component b.
    The product corresponding to the demulsifier according to the invention.
    20,280 g of component a, 79 g of component b (which corresponds to the mass ratio a ”to b in terms of 100% components 18: 1) and 280 g of di-H-butylformal are placed in a flask,
    25 equipped with a stirrer and nozzle for distilling off water, together with 11.1 g of a 35% by weight aqueous solution of formalin (which contains 11. 'g of formaldehyde - component b, which
    30 corresponds to its stoichiometric amount, counting on hydroxyl groups contained in components a and b). With stirring, 2.4 g of concentrated sulfuric acid are added (corresponding to 0.6 wt.% Sulfuric acid, counting the mass amount of a + b + c) and the reaction temperature is slowly raised to 160 ° C. while water is distilled off. After approximately 6 hours, the reaction is cooled to approximately 50 ° C and di-n-butyl formal is distilled off in a vacuum created by a water-jet pump (about 2000 Pa), with a repeated increase in temperature in the lower part to 160 ° C. After cooling to 100 ° C, 10 g are neutralized 30% sodium methylate solution. Get a brown viscous product, soluble ί; θ in organic solvents (e.g., xylene).
    Example 2. 540 g of component a according to example 1 and 30 g of η-nonylphenol formaldehyde resin ethoxylated with ethylene oxide, in an amount of 5 mol, similar to component b in example 1 in the form of a 90% by weight solution in xylene having a guide ~ ί
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    引用文献:
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    AU643324B2|1990-10-09|1993-11-11|Bp Chemicals Limited|Phenolic resin alkoxylates|
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    法律状态:
    优先权:
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