Claims
- 1. A process for the preparation of aqueous solutions of unsaturated quaternary ammonium salts corresponding to the following formula (I):
- H.sub.2 C=C(R.sub.3)--C(O)--A--R.sub.4 --N.sup.+ (R.sub.1)(R.sub.2)(R)X.sup.-
- in which:
- A is an oxygen atom or an NH group,
- R.sub.3 is a hydrogen atom or a methyl radical,
- R.sub.4 is a linear or branched alkyl radical with 1 to 6 carbon atoms,
- R.sub.1, R.sub.2 and R, which are different or identical, are an alkyl radical or an aryl radical,
- X is chosen from Cl, Br, I, CH.sub.3 -CO.sub.3 or CH.sub.3 -SO.sub.4, from at least one (meth)acrylic monomer (II) of formula H.sub.2 C=C(R.sub.3)--C(O)--A--R.sub.4 --N(R.sub.1)(R.sub.2) and from at least one quaternizing agent (III) of formula RX, in which formulae R, R.sub.1, R.sub.2 R.sub.3, R.sub.4, A and X have the above-mentioned meaning, in the presence of at least one polymerization inhibitor, in which process the reaction is carried out at a temperature of between 10.degree. C. and 80.degree. C., and in which
- (a) in a first stage, all or a part of the quaternizing agent (III) necessary for the is introduced into the reactor, this agent (III) being in the liquid state in the reaction conditions,
- (b) then, at least one (meth)acrylic monomer (II) is added, and
- (c) as soon as 0 to 30% of the stoichiometry of the (meth)acrylic monomer(s) has been introduced into the reactor, the remainder of quaternizing agent (III), the remainder of (meth)acrylic monomers and the water are added continuously and simultaneously until the desired concentration of unsaturated quaternary ammonium salts (I) has been obtained,
- (d) and, in the case where the quaternizing agent (III) is in the gaseous state at the reaction temperature, the reaction is carried out in the presence of oxygen and a pressure is applied in order that the quaternizing agent should be in the liquid state and, at the end of reaction, the pressure is gradually decreased to atmospheric pressure and simultaneously a ratio of volumetric flow rate of total gas at the exit of the reactor to the volumetric flow rate of oxygen introduced into the reactor which is lower than 100 is applied.
- 2. The process as claimed in claim 1, wherein, in the case (d) a ratio of volumetric flow rate of total gas at the exit of the reactor to the volumetric flow rate of oxygen introduced into the reactor which is lower than 50 is applied.
- 3. The process as claimed in claim 1, wherein the temperature is kept between 30.degree. and 60.degree. C. during the reaction.
- 4. The process as claimed in claim 1, wherein the introduction of the remainder of quaternizing agent (III), of the remainder of (meth)acrylic monomers (II) and of water in stage (c) is carried out as soon as 10 to 20% of the stoichiometry of the (meth)acrylic monomer(s) has been introduced in accordance with stage (b).
- 5. The process as claimed in claim 1, wherein the reaction is carried out at a temperature of between 10 and 80.degree. C. wherein,
- (a.sub.1) in a first stage, all or a part of the liquid quaternizing agent(s) (III) is introduced into the reactor,
- (b.sub.1) then, at least one (meth)acrylic monomer (II) is added, and
- (c ) as soon as 0 to 30% of the stoichiometry of the (meth)acrylic monomer(s) has been introduced into the reactor, the remainder of quaternizing agent (III) which is liquid at the reaction temperature, all or a part of the remainder of the methacrylic monomers (II) necessary for the reaction and all or a part of the water necessary for the reaction are added continuously and simultaneously, the total quantity of said quaternizing agent (III) which is liquid at the reaction temperature representing 0.1% to 99.9% of the stoichiometry in relation to said (meth)acrylic monomers (II),
- (d.sub.1) and then, the quaternizing agent(s) (III) gaseous at the reaction temperature, the remainder of the (meth)acrylic monomers (II) and the remainder of water are added continuously and simultaneously until the desired concentration of unsaturated quaternary ammonium salts (I) is obtained, the sum of the quantities of quaternizing agents added in stages (a.sub.1), (c.sub.1) and (d.sub.1) corresponding to a value equal to or higher than the stoichiometry in relation to the (meth)acrylic monomers (II), the reaction being then carried out in the presence of oxygen at atmospheric pressure or at a higher pressure, and wherein, during the reaction, at the end of reaction and during the application of atmospheric pressure a ratio of volumetric flow rate of total gas at the exit of the reactor to the volumetric flow rate of oxygen introduced into the reactor which is lower than 100 is applied.
- 6. The process as claimed in claim 2, wherein the temperature is kept between 30.degree. and 60.degree. C. during the reaction.
- 7. The process as claimed in claim 2, wherein the introduction of the remainder of quaternizing agent (III), of the remainder of (meth)acrylic monomers (II) and of water in stage (c) is carried out as soon as 10 to 20% of the stoichiometry of the (meth)acrylic monomer(s) has been introduced in accordance with stage (b).
- 8. The process as claimed in claim 3, wherein the introduction of the remainder of quaternizing agent (III), of the remainder of (meth)acrylic monomers (II) and of water in stage (c) is carried out as soon as 10 to 20% of the stoichiometry of the (meth)acrylic monomer(s) has been introduced in accordance with stage (b).
- 9. The process as claimed in claim 6, wherein the introduction of the remainder of quaternizing agent (III), of the remainder of (meth)acrylic monomers (II) and of water in stage (c) is carried out as soon as 10 to 20% of the stoichiometry of the (meth)acrylic monomer(s) has been introduced in accordance with stage (b).
Priority Claims (1)
Number |
Date |
Country |
Kind |
88/01635 |
Feb 1988 |
FRX |
|
Parent Case Info
This application is a continuation of application Ser. No. 07/754,317, filed Sep. 4, 1991, now abandoned, which is a continuation of Ser. No. 07/543,716, filed Sep. 7, 1990, abandoned.
PCT Information
Filing Document |
Filing Date |
Country |
Kind |
102e Date |
371c Date |
PCT/FR89/00036 |
2/2/1989 |
|
|
9/7/1990 |
9/7/1990 |
Publishing Document |
Publishing Date |
Country |
Kind |
WO89/07588 |
8/24/1989 |
|
|
US Referenced Citations (1)
Number |
Name |
Date |
Kind |
4745214 |
Hess et al. |
May 1988 |
|
Foreign Referenced Citations (1)
Number |
Date |
Country |
0250325 |
Dec 1987 |
EPX |
Continuations (2)
|
Number |
Date |
Country |
Parent |
754317 |
Sep 1991 |
|
Parent |
543716 |
Sep 1990 |
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