DE1717411B - - Google Patents

Description

1 719411

b) In the room where the mixing and reverse emulsification of the added water and oil phase takes place, the volume of the emulsion plus oil phase should always be larger than the volume of the non-emulsified water phase present in this space. The volume of reverse emulsion plus oil phase should be at least 1.5 times, preferably 5 to 3000 times the non-emulsified water phase in the mixing space.

c) The metering in of the water and oil phases should be carried out in such a way that they are fed in during the mixing process. Emulsification process on the way to the outlet opening have to wander through the agitating zone of the apparatus.

The presented reverse emulsion is expedient prepared in a discontinuous method beforehand in a stirred tank or in the apparatus itself.

Apart from the above-mentioned basic requirements, there are extensive freedoms in relation on the special construction of the emulsifying apparatus. This also applies to the overall dimensions as well as the Design of the stirrer and its speed. However, it is important to ensure that one is too intense active stirrer or too high stirring speed an already formed reverse emulsion, in particular at high contents of water phase, can destroy, while on the other hand a too weak active agitator is of course not usable for the production of a reverse emulsion, since then the shear forces are too weak to effect a fine distribution of the phases.

Appropriately, one chooses an upright cylindrical one provided with a lattice or tenon stirrer Vessel almost filled with inverted emulsion. Then the water and oil phases are dosed at the same time at the top of the vessel, stirring. The reverse emulsion is in the water plus The corresponding amount of oil phase is withdrawn from the bottom of the vessel.

An embodiment of such a device is illustrated in the drawing. This device consists of a cylindrical vessel 1, which is provided with a stirrer 2, the stirring blades 3

ίο and stirring rods 4 carries. At the top of the jar are feed lines 5, 6, 7 for the dosing of the components to be emulsified and at the lower end a drain pipe 8 with a tap 9 is attached. The vessel also has a vent pipe at its upper end 10 with a vent valve 11.

The reverse emulsions produced with the aid of the process according to the invention can, depending on the oil or water phase used and depending on the intensity of the stirring process, have a thin to creamy or creamy consistency. It is also possible to produce inverted emulsions in a heated apparatus by the process according to the invention.
The process is particularly suitable for the production of polymerizable, reverse emulsions, because in this way a continuous and, when working with a closed apparatus, air bubble-free mold filling of uniform quality can be achieved. According to the process, it is possible to activate the polymerization of the reverse emulsion to such an extent that rapid hardening in the molds is achieved without having to fear hardening in the stirring apparatus, as in the case of discontinuous work.

Of course, non-polymerizing reverse processes can also be used according to the process described Emulsions for the purpose of hydraulics or the formulation of active ingredients are produced.

example

Oil phase

ml / min.

Water phase

ml / min.

Stirrer
Kp / U

consistency

94% xylene
6% emulsifier 1

88% CCl ₄
4% polybutadiene
8% emulsifier 2

90% petrol
10% emulsifier 3

7% polyester resin *)
5% emulsifier 2
88% styrene

100
300

50
400

400
800
200
200
100
100

97V ₀ H ₂ O 100% H ₂ O

98% H ₂ O

96% H ₂ O

2% K ₂ S ₂ O ₈

2% NaOCOCH ₃ 96% H ₂ O

2V ₀ NaHSO ₃

2% NaOCOCH ₃

The aqueous solutions are metered in separately in equal parts 500
600

600
100

400
1600
600
800
600
800

2000
3500

1800
5000

5000
4000
3000
2800
2800
2000

creamy
creamy

thick cream thinly liquid

thin

creamy

creamy

creamy

creamy

stiff cream

The reverse emulsions of Examples 5 to 10 harden after several hours at 20 to 50 ^° C.

*) Polyester composed of 1 mol of maleic anhydride, 1 mol of phthalic anhydride, 1 mol of 1,2-propylene glycol, 1 mol of ethylene glycol; Molecular weight about 4000.

1 719411

Examples 1 to 10

The apparatus illustrated in the figure is first used with the emulsifier in question Oil phase filled to about 30 percent by volume. The metering is then carried out slowly and partially, with stirring Add about 60 to 65% water phase until a stable inverted emulsion is formed. Here is the The outlet cock is closed and the vent cock is open. Then the outlet cock is opened and closed the vent cock and simultaneously doses the water and monomer phases in the desired proportions a, the agitation speed is regulated so that a finely divided inverted emulsion arises. This drains from the outlet tap to the extent that the water and oil phases are added will.

As well as the originally submitted portion of the reverse emulsion taken from the apparatus is, the reverse emulsion of the composition determined by the dosage ratio can be at the outlet tap can be removed.

In the apparatus illustrated in the drawing, the conditions listed in the table were used reverse emulsions made.

Emulsifier 1: reaction product of 43 parts of diethylene glycol adipic acid polyester, 8.6 parts of polyethylene oxide, 4.3 parts of diphenylmethane-4,4'-diglycidether.

Emulsifier 2: graft polymer of polystyrene on polyethylene oxide with a polyethylene oxide content of about 10%.

Emulsifier 3: copolymer of 18 parts of oxypropyl methacrylate and 90 parts of dodecyl methacrylate.

1 sheet of drawings

Claims (1)

1 719411 1 2 Claim · ^{e 'ne to} 8 k ^{e enrte} emulsion from the same Components like the one to be manufactured is structured, Process for the production of inverted emulsions, at one end of the same the components sions, characterized in that the emulsion to be produced is fed continuously, but separately in a mixer provided with a stirrer, the latter emulsifying a re-emulsion within the optionally cylindrical mixing chamber and at the other end of the mixed-inverted emulsion, which continuously withdraws the finished emulsion from the same compo room, with components like the one to be produced, in front of the total volume of the emulsion and places, at one end of the same, the oily component flowing in the components always larger remains continuous as the emulsion to be produced, but io the volume of the inflowing aqueous fraction,
The process is carried out using an emulsified emulsion and a vessel provided with a stirrer at the other end, which is filled with the inverted emulsion continuously deposited in front of the mixing chamber. Into this draws, the total volume from the vessel placed in front of it, the water and oil phase of the emulsion to be produced and the inverse emulsion that is flowing in, which is the oily component 15, is simultaneously always greater than the volume of the inflowing desired volume ratio and after the aqueous portion. common passage through the powered agitator as a reverse emulsion in one of the volume of the supplied water and oil phase corresponding 20 amount discharged, with more oil phase + reverse emulsion than water phase in the stirring apparatus The invention relates to a method of production. reverse emulsions. Surprisingly, you can search for the invent-AIs Inverse emulsions are readily continuous emulsions according to the process called the water-in-oil type. Such emulsions are reverse emulsions with water contents of 60 sions have a continuous oil phase in which the up to 90 percent by volume by simultaneous unification The water phase is present in the form of tiny droplets dispersed in the two phases in the desired quantities. ratios obtained, while this is, for example, in the case of reverse emulsions with a content of the simultaneous combination of 1 part by volume of oil-water phase of less than 50 percent by volume, 30 phases with 7 parts by volume of water phase can be poured into one empty is not possible in the presence of suitable emulsifiers using a stirred tank. stirring of the components in the relevant quantities- The process is suitable for the production of conditions, although it is safe to use emulsions with a water phase content Aiming for a water-in-oil system is advisable, which is from 0.5 to 95 percent by volume (preferably 5 to Water phase slowly, partly in the submitted 35 85 percent by volume). Enter the emulsifier-containing oil phase with stirring. The reverse emulsion system is subject to The latter mode of operation is unavoidable if you do not have any in relation to the components that can be used safe reverse emulsions with contents of over general restriction, provided that these are fundamental Wants to produce 50 percent by volume, because the same-borrowed are suitable, the phases of a water-in-oil to show the early merging and mixing of both systems. Generally come as for example 20 parts by volume of emulsifier-containing oil phase oil phase all non-aqueous liquid systems in and 80 parts by volume of the water phase, none of the contaminated with the water phase to be used provides returned emulsion, but a dispersion of two-phase system capable of forming and their optionally some water phase containing oil phase surface-active properties the formation of a in the water phase. 45 does not prevent reverse emulsion. Due to the mode of operation shown so far, the same applies in a corresponding manner to the only the discontinuous production of reverse composition of the water phase, which is also a Emulsions, especially those with a water phase content, can be a multicomponent system, such as a solution of over 50 percent by volume, possible. or a dispersion. However, discontinuous work is not the case for the production of the reverse emulsion Continuous operation often used considerable emulsifiers, so-called vice versa we-disadvantages on how to use equipment and personnel to increase the emulsifiers, should be dissolved in the oil phase, inconsistent batches, easier soiling. This approach has proven to be the most appropriate of the approaches, frequent cleaning of the apparatus, have been proven, although the nature of the reverse work is relative lower capacity, etc. These disadvantages 55 the emulsifier and its use, provided that it make themselves especially in the production of polymer - always in sufficient quantity in the emulsifying sizable reverse emulsions noticeable, with system present, the continuous process the relatively long residence time of the reverse emul- not affected. sion in a batch-wise stirred tank For the operation of the emulsifying apparatus, (due to the necessary slow and 60 following measures proved to be particularly suitable, careful metering of the water phase) often to one premature thickening of the approaches. a) You should always so far with reverse emulsion The object of the invention is to ensure that the listed items are filled in such a way that the agitator is in this respect disadvantageous moves the known manufacturing process to swept emulsion and avoid that in the desired. This task is in a process 65 th quantitative ratio of incoming water and of the type described at the outset, according to the invention, there is an oil phase before and / or during their mixing solved by that one with a stirrer with the presented reverse emulsion in provided, possibly cylindrical mixing space are in contact.