IP Library Granted Patent US 9,884,299
Granted Patent B2
US 9,884,299 · App. 13/845,515 · Granted Feb 6, 2018

Process for the preparation of water-in-oil and oil-in-water nanoemulsions

Inventors: Lucilla Del Gaudio (San Donato Milanese, IT); Thomas Paul Lockhart (Lodi, IT); Alessandra Belloni (Cerro al Lambro, IT); Rossella Bortolo (Novara, IT); Roberto Tassinari (Novara, IT)
Assignees: ENI S.p.A.; POLIMERI EUROPA S.p.A.
B01F3/0811A61K9/1075B01F17/0085C09K8/524C09K8/528C09K8/54C10L1/328B01F2003/083B01F2003/0823
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Quick Facts
Patent No.
US 9,884,299
App. No.
13/845,515
Granted
Feb 6, 2018
Kind
B2
Abstract

Process for the preparation of a water-in-oil or oil-in-water nanoemulsion wherein the dispersed phase is distributed in the dispersing phase in the form of droplets having a diameter ranging from 1 to 500 nm, comprising: 1) the preparation of a homogeneous water/oil blend (I) characterized by an interface tension lower than 1 mN/m, comprising water in an amount of 30 to 70% by weight, at least two surface-active agents having a different HLB, selected from non-ionic, anionic, polymeric surface-active agents, said surface-active agents being present in such a quantity as to make the blend homogeneous; 2) the dilution of the blend (I) in a dispersing phase consisting of oil or water with the addition of a surface-active agent, selected from non-ionic, anionic, polymeric surface-active agents, the quantity of the dispersing phase and surface-active agent being such as to obtain a nanoemulsion having a HLB different from that of the blend (I).

Claims (25)

1. A low energy process for the preparation of an oil-in-water nanoemulsion wherein a dispersed phase is distributed in a dispersing phase in the form of droplets having a diameter ranging from 1 to 500 nm, said process consisting of:

diluting a

homogeneous water/oil blend (I) having an interface tension lower than 1 mN/m and comprising water in an amount of 30 to 70% by weight and at least two surface-active agents having a different HLB, said surface-active agents being selected from the group consisting of non-ionic surface-active agents, anionic surface-active agents, and polymeric surface-active agents, and said surface-active agents being present in said water/oil blend (I) an amount of from 5 to 50% by weight

in a

dispersing phase consisting of water and a surface-active agent selected from the group consisting of a non-ionic surface-active agent, an anionic surface-active agent, and a polymeric surface-active agent, the quantity of the dispersing phase and the surface-active agent being sufficient to obtain an oil-in-water nanoemulsion having an HLB higher than that of said homogeneous water/oil blend (I),

wherein during dilution a spontaneous and instantaneous phase inversion occurs, together with the formation of the nanoemulsion.

2. The process according to claim 1 , wherein, in the homogeneous blend (I), the weight ratio between the surface-active agents produces a HLB value higher than 8.

3. The process according to claim 2 , wherein the surface-active agents are selected from non-ionic surface-active agents and the weight ratio between the surface-active agents produces a HLB ranging from 10 to 15.

4. The process according to claim 2 , wherein the surface-active agents are selected from anionic surface-active agents and the weight ratio between the surface-active agents produces a HLB higher than 20.

5. The process according to claim 2 , wherein the weight proportion between the concentration of surface-active agents in the blend and the quantity of water/oil to be dispersed varies from 0.07 to 3.5.

6. The process according to claim 5 , wherein the weight proportion between the concentration of surface-active agents in the blend and the quantity of water/oil to be dispersed varies from 0.1 to 2.

7. The process according to claim 1 , wherein the surface-active agents having a different HLB are selected from non-ionic and polymeric surface-active agents.

8. The process according to claim 1 , wherein the surface-active agents having a different HLB are selected from the group consisting of a first surface-active agent selected from non-ionic lipophilic surface-active agents (type A), a second surface-active agent selected from non-ionic hydrophilic surface-active agents (type B), and a third surface-active agent selected from polymeric surface-active agents (type C), the composition of surface-active agents (A)+(B)+(C) having a HLB ranging from 8 to 16.

9. The process according to claim 8 , wherein the composition of surface-active agents (A)+(B)+(C) has a HLB ranging from 10 to 15.

10. The process according to claim 1 , wherein the surface-active agents having a different HLB consist of a non-ionic lipophilic surface-active agent of the group of esters of fatty acids with a HLB lower than 11, a non-ionic hydrophilic surface-active agent of the group of alkyl glucosides with a HLB higher than 11 and a non-ionic polymeric surface-active agent with a HLB varying from 4 to 14.

11. The process according to claim 1 , wherein the oil-in-water nanoemulsion is prepared by dissolving a hydrophilic surface-active agent in water and slowly adding the homogeneous blend (I) under stirring, said hydrophilic surface-active agent being selected from the group consisting of non-ionic surface-active agents and polymeric surface-active agents.

12. The process according to claim 1 , wherein the diluting of the blend (I) is performed at a temperature ranging from 5° C. to 60° C.

13. The process according to claim 1 , wherein the quantity of dispersing phase and the surface-active agent is sufficient to obtain a nanoemulsion having an HLB 0.5 units higher with respect to that of homogeneous water/oil blend (I).

14. The process according to claim 13 , wherein:

homogeneous water/oil blend (I) comprises non-ionic and polymeric surface-active agents,

the dispersing phase consists of water and a non-ionic surface-active agent selected from the group consisting of alkyl glucosides, and

the quantity of dispersing phase and surface-active agent is sufficient to obtain a nanoemulsion having a HLB at least 0.8-5 units higher than homogeneous water/oil blend (I).

15. The process according to claim 1 , wherein the oil for the preparation of the oil-in-water nanoemulsion is selected from the group consisting of linear hydrocarbons, branched hydrocarbons, and complex hydrocarbon blends.

16. The process according to claim 15 . wherein the oil is selected from the group consisting of dodecane, diesel, kerosene, soltrol, and mineral spirits.

17. The process according to claim 1 , wherein the water for the preparation of the oil-in-water nanoemulsion is selected from the group consisting of demineralised water, saltwater, and water containing additives.

Assignments (2)
CHANGE OF NAME Recorded Nov 21, 2025
From: POLIMERI EUROPA S.P.A.
To: VERSALIS S.P.A.
Reel/Frame 073256/0987 →
CONFIRMATORY ASSIGNMENT Recorded Nov 21, 2025
From: VERSALIS S.P.A.
To: VERSALIS OILFIELD SOLUTIONS S.R.L.
Reel/Frame 073662/0629 →
Priority Claims (1)
IT MI2006A0618 · Mar 31, 2006 · national
Continuity (2)
Division 12294552
Related Publication 20130209527A1 · Aug 15, 2013