DESC:FIELD OF INVENTION

The invention relates to a machine and a process in particular to a nano particle grinding.

PRIOR ART

The process of grinding consists of mainly 3 stages through which the invention/uniqueness is attained.

1. High shear blender.

Description:-
The ShearMaster is a high-speed mixing aggregate for intensive, time-saving mixing and dispersing of small quantities of product (1 - 10 l). It is equipped with a 1.1 kW electric drive. A frequency inverter allows infinite speed adjustment for the interchangeable mixing tools from 500 - 6000 min-1 or alternatively100 - 1200 min-1.

The mixing vessel, which can be a standard can or container, is easily exchangeable with the quick clamp device. To ensure the best possible vortex formation, the dissolver disk can be raised or lowered to the correct position by means of a linear motor in the IP model or a pneumatic cylinder in the Ex model. For monitoring and control of the operation, power consumption and speed are digitally displayed.

2. Positive displacement pump and circulation system:-

Description:-
These are the peril static pumps used for the circulation and delivery of product into the system and from the system. These are critical parts and need to be modified to suite various kinds of fluids that required to be transferred to and fro within the system and delivery of the product as well.

3. Multi-pass agitator bead mill:-

These bead mills provide effective de-agglomeration, size reduction and dispersion of the ultrafine particles in the emulsion after shear mixing as shown above. However, the tremendous surface area and surface energy that deliver the beneficial effects of ultrafine materials also prevent their easy dispersion into liquids. In addition, conventional technologies for dispersing powders into liquids are not sufficient for dispersing these tiny particles as discrete entities.

Producing stable suspensions or dispersions of ultrafine particles actually requires a comminuting process, such as that provided by a small-media mill. On an industrial level, this grinding of coarser particles into the nanometer range or dispersing agglomerated ultrafine primary particles is done with a bead mill, even though the high energy and bead speeds typically required can lead to material contamination or the destruction of the crystalline structure of the particle.

It has been discovered that mills using very fine media beads, in the range of 70-125 µm, can economically grind materials into the nanometer range. It has also been discovered that unique mill designs using ultra-fine grinding beads of 30-50 µm in size offer an effective solution for dispersing these particles with significantly improved process efficiency.

One limitation in the process up to this point has been a lack of knowledge concerning scalable industrial equipment that uses these small beads. Additionally, this method is not widely accepted due to the difficulty of handling the small grinding beads.

OBJECT OF THE INVENTION:-

1. The object of the present invention is to provide a grinding process for forming nano particle emulsion to reduce the cost for operation, prevent the contamination and abrasion of grinding-media, and achieve high milling efficiency for the natural essential oils and oleoresins.

2. Another object of the present invention is to provide a grinding process for forming nano particle emulsion to disperse the natural dye at a nano-scale (<1000 nm) so as to increase the color saturation and distribution of colors.

3. Another object of the present invention is to provide a pigment dispersion, wherein the pigment particles are in a nano-scale and well dispersed to increase the color saturation.

4. Another object of the present invention is to provide 1.5 to 2 times or more solubility and reduce the additives and thereby also reduce the dosage in the application.

5. Another object of the present invention is to provide higher surface area to the particles forming the emulsion and thereby increase the biological availability to a proportionate extent of the designed application.

SUMMARY OF INVENTION

A grinding process for forming a slurry of ultrafine particles in the range from 100 to 1000 nanometer, consists of the following steps: forming a mixture by mixing a matrix, a dispersant and dispersing media together; adding a pre-treated grinding-media into the mixture; Wherein the grinding-media are zirconium oxide beads With an average particle diameter of less than 2mm; milling or grinding the mixture; and separating the grinding-media from the mixture to get an emulsion of nano particles. A natural dye dispersion produced from the grinding process is also included within the scope of the invention.

PROCESS FLOW DIAGRAM
Figure 1 – Illustrates process flow diagram.
Figure 2 - Higher Bio availability proof diagram

DRAWINGS OF THE INVENTION
PART NO PART NAME
1. Material Powder
2. Raw Material Silo
3. High-speed pre-dispersing Tank
4. Feed Tank
5. Single Screw Pump
6. Separator
7. Head Tank
8. Wet Ball Mill
9. Flow meter
10. Slurry Tank
11. Single Screw Pump
12. Material Returning Tube
13. Semi-finished Product Slot
14. Single Screw Pump
15. Viscosity Adjusting Tank
16. Single Screw Pump
17. Pipeline Pressure Screen
18. Finished Product Slot

DESCRIPTION OF THE INVENTION

To achieve the object, the grinding process for forming an emulsion of nano particles comprises the following steps:

a. forming a mixture by mixing a matrix, a dispersant and a dispersing media together; adding a pre-treated grinding-media into said mixture; Wherein said grinding-media are zirconium beads With an average particle diameter of less than 1000 nano meter; milling or grinding said mixture; and separating said grinding-media from said mixture to achieve a final emulsion of nano particles.

b. A pigment dispersion comprising : 0.1 to 95 Wt % of a pigment With an average particle diameter of less than 1000 nm; 0.1 to 25 Wt % of dispersant; and 30 to 90 Wt % of Water; Wherein said active ingredient pigment is formed by milling or grinding a mixture of a matrix, said dispersant and a dispersing media with zirconium oxide beads having an average particle diameter of less than 2mm until the average particle size of the matrix particle is less than 1000 nm.

c. Other objects, advantages, and novel features of the invention will become more apparent from the following detailed description when taken in conjunction with the attached drawings and specification sheets.

In one of the embodiments, the grinding process for preparing an emulsion of nano particles comprises of the following steps.

The first step is to prepare/form a mixture by mixing a matrix, a dispersant and dispersing media together. Thereafter adding a pre-treated grinding-medium into said mixture. The said pre-treated grinding-medium are glass beads. These glass beads shall have an average particle diameter of less than 2mm. Thereafter the said mixture is either milled or ground until the average particle diameter of the said matrix is less than 1000 nm. Thereafter separating the grinding-medium from said mixture to obtain an emulsion or liquid dispersion of nano particles.

In another embodiment, said matrix is selected from the group consisting of natural dyes, and pigments, crystalline organic molecules, polymers, or medicine powders of natural origin from spices, herbs or other botanicals.

In another embodiment, the said dispersant is selected from the group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and polymeric surfactants and a mixture thereof.

Furthermore the said pre-treated grinding-medium is generally sieved out and preferred method is by an overflow system. The average particle diameter of said grinding-medium shall range between 0.2 to 2mm in size and the density of said grinding-medium shall be in the range from 3.3 to 4.2 kg/liter. Most preferably the grinding-medium shall be in a ball-shape.

In another embodiment, the said milling or grinding is carried out in a mill having a stainless steel mixing tank and a stirring blade.

In another embodiment, the said mill may be is an airier mill, a roller mill, a ball mill, an agitator mill, a vibratory mill, a planetary mill, a sand mill or a bead mill.

The said milling or said grinding may be achieved in a batch mode, a continuous mode or a semi-batch mode.

Furthermore, the said slurry or emulsion of nano particles is used in the above mentioning manufacturing process of dispersion of the active ingredients for food, feed and Nutraceutical or pharmaceutical purpose.

As per the other objects of the invention, the invention arise at an emulsion dispersion comprising of
a. 0.1 to 95wt% of an emulsion having an average particle diameter of less than 1000nm.
b. 0.1 to 25 wt% of dispersant and
c. 30 to 90 wt% of water wherein said emulsion is formed by melting or grinding a mixture of a matrix, said dispersant and a dispersing medium with grinding medium comprising glass beads having an average particle diameter of less than 2mm.

The above said dispersant is selected from the group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and polymeric surfactants and a mixture thereof.

In the invention there is a disclosure of the grinding mill for preparing an emulsion of nano particles of size less than 1000 nm, wherein the said mill comprises :
- a contoured grinding chamber,
- a contoured blade in the chamber and
- a plurality of grinding beads having plurality of diameters

The grinding chamber is contoured such that it has plurality of paths and slots accommodated within a hollow shaft and the flow of the product and contact with the beads are filtered through a stainless steel cylindrical meshed shell and the contour of the said blades are such that it forms a peg type system in hollow shaft. In the above grinding mill, the grinding beads used in the process shall have diameter in the range 0.2 to 4 mm to achieve the objects of the process and to suit the grinding mill designed herein above.

COMPARISON OF PROCESSES:-

Sl. no. Typical Process step known in prior art Revised Process Step Difference Point of Claim in the invention
1 Active ingredient in extracted emulsion or dispersion or powder form in a blend With minimal application of surfactant, crude with Crude is taken with ideal level of active ingredient suitable for ultrafine grinding
2 Manual or machine assisted blending Shear mixing and blending in the netzsch make Mastershear New process of pre-blending and sheer mixing is applied
3 Homogenizer in standard form Ultrafine grinding in Netzsch LMZ model agitator bead mill and planatory mill The particles in the emulsion is ground to nano sized particles Application of LMZ mill of conversion of particles in emulsion to nano size range
4 No process Preparation of final blend to standardized form using surfactants and emulsifiers Addition of final blending step

COMPARISON OF MACHINERY:- (MACHINE COMPARISON)

Sl. no. Typical machine known in prior art configuration and setup Revised machine configuration and setup Difference Point of Claim in the invention
1 Sheer mixing with single layer wheel Shear mixing with contour specific to spice emulsion Specific contour blade Selection and use of multi contour blades
2 Beads size, material Zirconimum oxide bead for spice milling with multi dia ranging from 0.2 to 2mm Specific size and material of construction of grinding tool Size and material of construction of beads
3 Profile of material flow and grinding surface single contour profile and slot Multi-pass varying contour profile with slots and path for material passing and grinding with minimum destruction to the actives Selection of profile and milling path configuration with specific, velocity, flow rate, pressure and temp. Use of specific profile for the milling surface and process parameters
4 Material of construction Specifically SS316 in combination with Zirconium oxide beads Other combinations not specific to spices

COMPARISON OF PRODUCT BASED ON GENERAL CHARACTERISTICS:-

Sl. no. Parameters for comparison Prior art method or normal extraction process result Invented new process results in the products Point of Claim in the invention
1 Particle size Above 2000 micro meter 100 to 1000 micro meter Lower particle size and higher surface area that increases the utility
2 Zeta potential Depends on blend Can prepare to a specific Better dissolution and stability
3 Colour hue Varying depending on the blend and shows settling tendency Standardized and comparatively better to same spec of normal More integral blend throughout the section of the container due to imparting Brownian phenomena
4 Binding strength Depends on surfactant With minimum surfactant better binding can be seen Lower usage of surfactant and hence higher ratio of dosage can be achieved.
5 Bio activity Depending on blend With modified rheological properties, higher activity is recorded to a level of 200%
Refer fig. 2 Possibility to consider as natural therapeutic ingredients for certain medicinal applications
6 Resistance against propagation of tumour cells The measured activity with respect to resistance against propagation of tumour cells was found to be more in this new format.
7 Dosage The enhanced activity was comparable to that of cyclophosphamide a known anti-tumor drug which was given at a dosage of 25mg/kg,
8 Tumour development The product produced in this machine in water and oil soluble form had reduced the tumor development induced by Dalton’s Lymphoma Ascites tumor cells in mice.
9 Absorption Vextrano Curcumin exhibited significantly higher absorption (nearly two fold) and AUC as compared to the Oleoresin Curcumin.

Concise report of evaluation
Pharmacokinetic Parameters

Vextrano

Oleoresin
Parametres Values Parameters Values
T1/2 1.98 h T1/2 0.90 h
Cmax 0.33341 µg/ml Cmax 0.167 µg/ml
tmax 45 min tmax 30 min
MRT 5.55 h MRT 5.89 h
AUC(o-t) 0.720688 AUC(o-t) 0.438898

SOME OF THE NOVELTY FEATURE ARE

A grinding process for preparing an emulsion of nano particles, comprising the following steps:

(a) forming a mixture by mixing a matrix, a dispersant and dispersing media together;

(b) adding a pre-treated grinding-medium into said mixture; wherein said pre-treated grinding-medium are glass beads having an average particle diameter of less than 2mm

(c) milling or grinding said mixture until the average particle diameter of the said matrix is less than 1000 nm; and

(d) separating grinding-medium from said mixture to obtain an emulsion or liquid dispersion of nano particles.

In another aspect, the said matrix is selected from the group consisting of natural dyes, and pigments, crystalline organic molecules, polymers, or medicine powders of natural origin from spices, herbs or other botanicals.

In another aspect, the said dispersant is selected from the group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and polymeric surfactants and a mixture thereof.

In another aspect, the said pre-treated grinding-medium is sieved out by an overflow system.

In another aspect, the average particle diameter of said grinding-medium ranges from 0.2 to 2mm.

In another aspect, the density of said grinding-medium ranges from 3.3 to 4.2 kg/liter

In another aspect, the said grinding-medium is in a ball-shape.

In another aspect, the said milling or grinding is carried out in a mill having a stainless steel mixing tank and a stirring blade.

In another aspect, the said mills an airier mill, a roller mill, a ball mill, an agitator mill, a vibratory mill, a planetary mill, a sand mill or a bead mill.

In another aspect the said milling or said grinding is achieved in a batch mode, a continuous mode or a semi-batch mode.

In another aspect the said slurry or emulsion of nano particles is used in the manufacturing of dispersion of the active ingredients for food, feed and Nutraceutical or pharmaceutical purpose.

The invention further discloses an emulsion dispersion comprising:
a.0.1 to 95wt% of an emulsion having an average particle diameter of less than 1000nm.
b. 0.1 to 25 wt% of dispersant and
c. 30 to 90 wt% of water wherein said emulsion is formed by melting or grinding a mixture of a matrix, said dispersant and a dispersing medium with grinding medium comprising glass beads having an average particle diameter of less than 2mm.

The emulsion dispersion mentioned above includes dispersant selected from the group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and polymeric surfactants and a mixture thereof.

The invention further discloses grinding mill for preparing an emulsion of nano particles of size less than 1000 nm, wherein the said mill comprises :
- a contoured grinding chamber,
- a contoured blade in the chamber and
- a plurality of grinding beads having plurality of diameters

In another aspect the grinding chamber is contoured such that it has plurality of paths and slots accommodated within a hollow shaft and the flow of the product and contact with the beads are filtered through a stainless steel cylindrical meshed shell.

In another aspect the contour of the blade is such that it is peg type system in hollow shaft.

In another aspect the said grinding beads having diameter in the range 0.2 to 4 mm.

All of these aspects and embodiments are merely given for sake of easy understanding and shall not limit the scope of invention.

Although the present invention has been disclosed and described in relation to preferred embodiments, it is stated that other modifications and variations can also be made without departing from the spirit and scope of the invention. All such variations and modifications are within scope of invention.
,CLAIMS:1. A grinding process for preparing an emulsion of nano particles, comprising the following steps:

(a) forming a mixture by mixing a matrix, a dispersant and dispersing media together;

(b) adding a pre-treated grinding-medium into said mixture; wherein said pre-treated grinding-medium are glass beads having an average particle diameter of less than 2mm

(c) milling or grinding said mixture until the average particle diameter of the said matrix is less than 1000 nm; and

(d) separating grinding-medium from said mixture to obtain an emulsion or liquid dispersion of nano particles.

2. The process as claimed in claim 1, wherein said matrix is selected from the group consisting of natural dyes, and pigments, crystalline organic molecules, polymers, or medicine powders of natural origin from spices, herbs or other botanicals.

3 The process as claimed in claim 1, wherein said dispersant is selected from the group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and polymeric surfactants and a mixture thereof.

4 The process as claimed in claim 1, wherein said pre-treated grinding-medium is sieved out by an overflow system.

5 The process as claimed in claim 1, wherein the average particle diameter of said grinding-medium ranges from 0.2 to 2mm.

6. The process as claimed in claim 1, wherein the density of said grinding-medium ranges from 3.3 to 4.2 kg/liter

7. The process as claimed in claim 1, wherein said grinding-medium is in a ball-shape.

8. The process as claimed in claim 1, wherein said milling or grinding is carried out in a mill having a stainless steel mixing tank and a stirring blade.

9. The process as claimed in claim 8, wherein said mill is an airier mill, a roller mill, a ball mill, an agitator mill, a vibratory mill, a planetary mill, a sand mill or a bead mill.

10. The process as claimed in claim 1, wherein said milling or said grinding is achieved in a batch mode, a continuous mode or a semi-batch mode.

11. The process as claimed in claim 1, wherein said slurry or emulsion of nano particles is used in the manufacturing of dispersion of the active ingredients for food, feed and Nutraceutical or pharmaceutical purpose.
12. An emulsion dispersion comprising:
a. 0.1 to 95wt% of an emulsion having an average particle diameter of less than 1000nm.
b. 0.1 to 25 wt% of dispersant and
c. 30 to 90 wt% of water wherein said emulsion is formed by melting or grinding a mixture of a matrix, said dispersant and a dispersing medium with grinding medium comprising glass beads having an average particle diameter of less than 2mm.
13. The emulsion dispersion as claimed in claim 12, wherein said dispersant is selected from the group consisting of anionic surfactants, cationic surfactants, nonionic surfactants and polymeric surfactants and a mixture thereof.

14. A grinding mill for preparing an emulsion of nano particles of size less than 1000 nm, wherein the said mill comprises:
- a contoured grinding chamber,
- a contoured blade in the chamber and
- a plurality of grinding beads having plurality of diameters

15. The grinding mill as claimed in claim 14, wherein the grinding chamber is contoured such that it has plurality of paths and slots accommodated within a hollow shaft and the flow of the product and contact with the beads are filtered through a stainless steel cylindrical meshed shell.

16. The grinding mill as claimed in claim 14, wherein the contour of the blade is such that it is peg type system in hollow shaft.

17. The grinding mill as claimed in claim 14, wherein the said grinding beads having diameter in the range 0.2 to 4 mm.