Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F2/00—Processes of polymerisation
  • C08F2/32—Polymerisation in water-in-oil emulsions

Definitions

• the present invention relates to a dispersant used when performing a reversed-phase suspension polymerization by adding a water-soluble aqueous diethylene unsaturated monomer solution to a polymerization-inactive and hydrophobic solvent. It is a dispersant for reversed-phase turbid polymerization that can stably maintain a polymerization system.
• dispersants used in reverse-phase emulsion polymerization of water-soluble ethylenically unsaturated monomers include: sorbitan monostearate, sorbitan monooleate, and ethoxylated aliphatic alcohol.
• Non-ionic surfactants such as mid and dariscelin fatty esters are known (JP-B-54-30710, etc.).
• a water-treated maleic acid product of a resin having an aryl (A11 yl) group, and a polymerization charge having a lipoxyl group having an affinity for an organic solvent for example, a water-treated maleic acid product of a resin having an aryl (A11 yl) group, and a polymerization charge having a lipoxyl group having an affinity for an organic solvent.
• High molecular compounds such as lipophilic textile derivatives are known (JP-A-57-74309).
• the former group non-ionic surfactant
• the resulting polymer becomes fine particles, which causes problems such as generation of dust in the separation and drying steps.
• the resulting polymer is in the form of small agglomerates, and although the above-mentioned disadvantages can be improved, the polymer particles and the wall of the polymer are stirred or mixed during the polymerization operation. It is inevitable that a large part of the reacted fumer will be lost as unusable polymerized plant deposits due to the stickiness caused by the tomato. Generally, removing the polymerized / adhered matter of the water-soluble ethylenically unsaturated herb requires a great deal of effort from dogs, resulting in efficient production of granular polymer.
• the present Kiyoshi et al. Found that using a polymer having a specific structure as a fu position repeatedly as a dispersant in reverse-phase turbidity polymerization provided fine particles.
• the present inventors have found that a small granule containing no polymer can be obtained stably, and have completed the present invention.
• the present invention provides: (CH CH-R 3 , N
• the combination c with R z , R 2 ) is (H, .H), (H, CH 3 ), (H, C 2 oH 5 ), (CH 3 , C 2 H 5 ) (H, It is any one of the group consisting of a straight-chain or branched alkyl group having 6 or more carbon atoms) and (H, an alkoxyethyl group having 6 or more carbon atoms).
• R 3 and R each represent H or a straight or branched alkyl group having 6 or more carbon atoms or an alkoxyethyl group having 6 or more carbon atoms.
• n represents an integer of 1 to 3.
• the dispersant for reversed-phase suspension polymerization of the present invention is a dispersant for reversed-phase suspension polymerization, which comprises a balance between a polar amide moiety and a nonpolar alkyl or alkoxyethyl moiety. Good performance as an agent.
• the reversed phase dispersant of the present invention can be produced, for example, by the following method. That is,
• a polymer of at least one N-Bull ring amide represented by is converted to a «-olefin or carbon having 6 or more carbon atoms by using a peroxide compound. It can be produced by alkylation or alkoxyethylation with an alkyl vinyl ether having an alkyl group of several or more. More specifically, a polymer of N-Bull cyclic amide is dissolved in a suitable solvent, for example, n-hexano-one-mole, n-amirea-reco-one-mele, methicole-soft-birketone, etc.
• a portion (unit) other than the above-mentioned repeated position may be included as long as the performance as a dispersant for the turbid polymerization is not hindered.
• the monomer capable of constituting such a portion include: unsaturated monocarboxylic acid ester such as alkyl methacrylate or alkyl acrylate having an alkyl group having 6 or more carbon atoms, dianolequinolate, Non-encapsulated rosin compounds such as dianolequinolefumarate and diaquinolose tancone, monomers having an aromatic ring such as propylene diester, styrene, and alkylstyrene, alkyl vinylinolenate, Examples thereof include anolex lesbininolates and mixtures thereof. "-Refin can also be used.
• the ⁇ -vinyl cyclic amide polymers which can be used in the production of the dispersant for reversed phase polymerization of the present invention by the above-mentioned method include ⁇ -vinyl viridone and ⁇ -Bulle-5. -Alkylpyrrolidone, ⁇ -vinylbiperidone, ⁇ -vinyl-6-alkylbiperidone, ⁇ -bulcaprolactam, ⁇ -bi Polymers of nil-7-alkynorecaprolactam.
• an N-vinylpyrrolidone polymer is preferable because a poly (vinylpyrrolidone) having a market ⁇ can be used as it is.
• These polymers of ⁇ -Bull ring amide can be suitably used as long as they have an average molecular weight of 1,000 to 100,000, more preferably 5,000 to 500,000.
• any straight or branched one having 6 or more carbon atoms may be used as the orifice that can be used in the above method. Numbers between 10 and 20 are more preferred. If the number of carbon atoms is smaller than 6, the produced dispersant has insufficient oil solubility and loses its performance as a dispersant.
• Examples of the olefin having 10 to 20 carbon atoms include eicosene, and commercially available ones can be used.
• Alkyl vinyl ethers that can be used in the above method include any alkyl vinyl ether having an alkyl group having 6 or more carbon atoms. 9
• the alkyl group has less than 6 carbon atoms, the produced dispersant has insufficient oil solubility and cannot function as a dispersant.
• the appropriate amount of the dispersant to be used is usually 0.0 to 10% by weight based on the polymer. %, Preferably 0.05 to 5.0% by weight.
• any solvent having polymerization inertness and water-insoluble property can be used. is there.
• aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons or mixed solutions thereof having a point of 30 to 200 are preferred.
• it is especially useful for San, benzene, toluene or a mixed solvent thereof is preferably used.
• water-soluble ethylenically unsaturated polymer which can be polymerized by reverse phase suspension polymerization to which the dispersant of the present invention is applied
• various compounds can be mentioned.
• a water-soluble crosslinking agent having two or more polymerizable unsaturated groups such as, for example, methylene bisacrylinoleamide, or a functional group of an ethylenically unsaturated fumer may be used.
• a water-soluble cross-linking agent having two or more functional groups that can react with, for example, ethylene glycol diglycidyl ether, crosslinks during (co) polymerization of the above monomer or after polymerization ⁇ It is also possible to react.
• the monomer concentration of the aqueous monomer solution in the present invention can be changed in a wide range, but generally 15 to 80% by weight is preferable.
• the ratio of the amount of the aqueous solution of fumer and the amount of the polymerization-inactive and hydrophobic solvent can be changed over a wide range, but usually, the ratio by volume is 1: 1 to 1: 1: A range of 4 is preferred.
• a water-soluble radisol polymerization initiator such as a peroxide, a hydroperoxide, or an azo compound is used in a known amount. 6/05792
• polymerization initiators can be used as a mixture of two or more kinds.Furthermore, redox polymerization initiation is performed by adding chromion, sulfite, hydroxylamine, hydrazine and the like. It can also be used as an agent.
• the dispersant for reverse phase polymerization of the present invention has a polar amide moiety and a nonpolar alkyl or alkoxymethyl group moiety, and is suitable for reverse phase polymerization.
• the dispersant is regularly oriented at the oil-water interface and stabilizes both interfaces, so it is considered that the reversed-phase suspension polymerization system is stably maintained.
• the reaction was performed at 5-130'c for 20 hours. After an additional 2.5 g of peroxide was added, the reaction was performed for 10 hours. The n-hexanol and unreacted oil were distilled off under reduced pressure to obtain a pale yellow viscous liquid. Its IV was 5.6, which was dissolved in cyclohexane.
• Polysodium acrylate was obtained.
• the amount of the dressing in ⁇ was 0.5 g.
• Example 1 polymerization was performed using Dispersant B, Dispersant C, Dispersant D, and Dispersant E instead of Dispersant A, respectively.
• Table 1 shows the center particle size and the amount of the attached poly (sodium polyacrylate).
• Example 1 25 g of sodium vinyl sulfonate was used instead of acrylonitrile as the aqueous solution of ethylenically unsaturated fumer, and this was ion-exchanged.
• the monomer dissolved in 75 g of water replacement was used, small particles of sodium polyvinylsulfonate having a center particle diameter of 130 to 350 m were obtained.
• the amount of deposits in the area was 0.8 g.
• the polymerization was carried out according to Example 1. However, when 1.2 g of sorbitan monostearate was used in place of dispersant A, only a particulate polymer having a center particle size of 30 to 7.0 ⁇ m was obtained. The amount of deposits in the reaction tank was 0.9 g.
• the productivity can be significantly improved. it can.
• the dispersant for reverse-phase turbid polymerization of the present invention when used, the polymerization of the polymer into a polymerization apparatus or a stirrer can be performed. Since the amount of adhesion can be extremely small, the polymerization apparatus can be used continuously.

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• Chemical & Material Sciences (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Health & Medical Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Polymerisation Methods In General (AREA)
• Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)

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Citations (2)

• 1985
  • 1985-04-05 JP JP7241885A patent/JPS61231004A/ja active Pending
• 1986
  • 1986-04-04 GB GB8624298A patent/GB2181140B/en not_active Expired
  • 1986-04-04 WO PCT/JP1986/000162 patent/WO1986005792A1/ja active Application Filing
  • 1986-04-04 NL NL8620116A patent/NL8620116A/nl not_active Application Discontinuation
  • 1986-04-04 DE DE19863690157 patent/DE3690157T1/de not_active Withdrawn

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