JPH0341197A - Coated perfume particle - Google Patents

Abstract

PURPOSE: To obtain coated perfume particles discharging particles in an automatic washer or a washing dryer to release perfume by dispersing perfume throughout a water-insoluble polymer carrier substance and applying a fragile coating substance on the surfaces of the particles.

CONSTITUTION: Coated perfume particles has an average particle size of about 350 μm or less at a time of coating and contain about 5-70% of perfume dispersed in about 30-95% of a water insoluble polymer carrier substance with a mol.wt. of about 100-30,000, an m.p. of about 37-190°C and a hardness value of about 0.1-15 thereof and have a fragile coating substance on the outer surfaces thereof. As the carrier substance to be used, polyethylene, polyamide, polystyrene, polyisoprene, polycarbonate or polyester can be designated. The water insolubility of the coating substance may be imparted by the crosslinking of gelatin-gum arabic in an aldehyde or other known gelatin curing agent suitable after adhesion. The polymerization of a urea-formaldehyde precondensate at a time of an encapsulating process causes water insolubility.

COPYRIGHT: (C)1991,JPO

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to perfume particles comprising a perfume dispersed within a water-insoluble low molecular weight polymer material and encapsulated with a friable coating. Such coated particles are useful, for example, in cleaning and fabric conditioning compositions.

BACKGROUND OF THE INVENTION The present invention is based on the concept of controlled perfume release, ie, perfume release at predetermined times under conditions that will achieve the desired perfume effect. In general, this is a very old idea and a variety of methods have been developed to achieve this goal, from the simple idea of putting perfume in candles to the complex technology of microencapsulation.

One aspect of the concept of controlled release of perfume is to provide a slow release of perfume over an extended period of time. This is commonly accomplished by blending the perfume with a substance that will essentially "trap" the perfume so that small amounts of perfume are released over a period of time. The use of high molecular weight polymeric materials formulated with fragrance to provide a controlled release of fragrance over a period of time
Known. For example, combining a fragrance with a controlled release vehicle,
U.S. Pat. No. 4,184,099, European Patent Application No. 0 028 118 and U.S. Pat. No. 4,110,261 which teach forming a combination into an air fresh substitute solid product. reference.

Fabric laundering also involves controlled release of fragrances.

Application of this concept makes it possible to delay or prevent the release of fragrances through long-term storage.

Such a concept also allows much less fragrance to be used in the product since much less fragrance is wasted.

Flavor preservation over storage time can be achieved in a variety of ways. The perfume can be part of the packaging for the composition. The fragrance can be combined with the plastic used to make the bottle, or the fragrance can be combined with the polymer used to coat the cardboard packaging composition as disclosed in U.S. Pat. No. 4,540,721. Can be mixed with substances and products. In either method, the perfume is released from the polymer matrix over a period of time.

The perfume/controlled release agent may also be in the form of particles incorporated into the laundry composition. One method taught to accomplish this goal is U.S. Pat. No. 4,209,41
No. 7, U.S. Pat. No. 4,339,356 and U.S. Pat. No. 3,576,760, perfumes are combined with water-soluble polymers and formed into particles;
It is added to laundry compositions.

The perfume may also be adsorbed onto a porous carrier material, which may be a polymeric material. For example, UK Patent Section 2,066
．． See specification No. 839. These methods may also be used to mask unpleasant odors in compositions or to protect fragrances from deterioration by harsh ingredients in laundry compositions. Since the perfume is released upon hydration of the polymer, such a method would confer these benefits only to dry powder, or granular type compositions. These methods thus provide perfume aroma benefits upon opening of the product package and upon loading into the cleaning equipment. These benefits are desirable, but the undiluted, undiluted, unchanged fragrance at the end of the washing process imparts the desired fragrance to the fabric! It would be even more desirable to have a method that allows for the delivery and release of fragrance to a fabric of:1.

Of course, one way to accomplish this goal is to place the fragrance into the product that goes directly into the dryer.

In this method, perfume is delivered to the fabric in a dryer cycle. Such a method is described in U.S. Pat.
No. 1,495 and U.S. Pat. No. 4,636,330. Both teach forming perfume into particles with a carrier. These particles are then formulated into a composition that is applied to the fabric prior to entering the dryer or prior to fabric line drying.

A more desirable method for delivering perfume to a laundered fabric would be one that provides protection of the perfume throughout the washing process and therefore delivery of the perfume to the fabric in an essentially light state.

Such methods should allow prevention of dilution, deterioration or loss of perfume during the wash cycles of the laundry process. This is done by utilizing a system that releases the perfume during the drying process or after the perfume has been delivered to the fabric. Preventing perfume release during the washing process involves a very different and more difficult technique. Such protection must not only be stable under the thermal elevated conditions of the cleaning process, but also be resistant to degradation by water and other harsh chemicals in the cleaning process, such as bleaches, enzymes, surfactants, etc. Must be stable.

One method developed to provide these benefits is perfume microencapsulation. Here, the perfume consists of a capsule core completely coated with a substance which may be a polymer. U.S. Pat. No. 4,145.184 and U.S. Pat. No. 4,234,627 teach the use of tough coating materials that essentially inhibit perfume diffusion. The perfume is delivered to the fabric by microcapsules and then released by rupture of the microcapsules, such as that which would occur in the case of manipulation of the fabric.

Another method of perfume delivery involves providing protection of the perfume through the wash cycle and releasing the perfume under elevated heat conditions in a dryer. U.S. Pat. No. 4,096,072 discloses a method for delivering fabric conditioning agents to fabrics through wash and dry cycles by particles containing hydrogenated castor oil and fatty quaternary ammonium salts. teaching. Perfume may be incorporated into these particles. However, it is not clear whether the perfumes thus incorporated are released in the wash cycle or, more preferably, are carried in the particles to the dryer and released there as the particles soften.

U.S. Pat. No. 4,402,856 teaches a microencapsulation technique that involves the formulation of a shell material that will allow diffusion of perfume from the capsule only at temperatures that are: This allows maintenance of the perfume particles throughout storage and additionally through washing cycles. The particles adhere to the fabric and are carried over to the dryer. Diffusion of perfume from the capsule then occurs only under the elevated temperature conditions of the dryer. These particles are made from gelatin, an anionic polymer and a hardening agent.

US Pat. No. 4,152,272 teaches incorporating perfume into wax particles to protect the perfume through storage in dry compositions and through the laundering process. The perfume then diffuses through the wax matrix of particles on the fabric under the elevated heat conditions of the dryer.

It would be desirable to provide compositions containing corrugated bodies and perfume particles that can be incorporated into dry granular or powder compositions and provide long-term storage stability.

It would be desirable to provide a method for delivering a wide range of fragrance materials to fabrics or other surfaces during cleaning or fabric or fiber conditioning processes.

Having a scented cleaning or conditioning composition that will provide improved product odor, improved fragrance odor emitted during the cleaning process, and improved odor and intensity of fragrance delivered to the surface to be cleaned. would be most desirable.

It would be particularly desirable to provide perfumed particles that are stable in fluid compositions but release perfume during use.

SUMMARY OF THE INVENTION The present invention provides coatings that, when coated, have an average size of about 350 microns or less (preferably an average size of about 150 microns or less, most preferably 40 to 1
a water-insoluble polymeric carrier material having a molecular weight of about 100 to about 30,000, a melting point of about 37°C to about 190°C, and a hardness value of about 0.61 to about 15.
Includes perfume particles characterized by comprising about 5% to about 70% perfume dispersed in 0% to about 95%, said particles having a friable coating on their outer surface (herein ""Size" means the average particle size in the case of substantially spherical particles and the maximum diameter or dimension size in the case of non-spherical particles)
.

Particle sizes larger than this may be lost from the surface to which it is attached and do not provide sufficient relatively large surface area to release perfume at the desired rate.

Also, particles larger than those specified herein may be undesirably visible on the treated surface. Particles at the lower end of the range tend to adhere well to the treated surface, but tend to release perfume quite quickly.

Typically, the particles of the invention are characterized by a coating comprising up to 20% by weight of the perfumed particle. For general use in fabric laundry and conditioning compositions, the coating typically contains 1 to 1 of the perfumed particles.
It constitutes 0% by weight.

Preferred particles of the invention are those in which the friable coating is substantially water-insoluble. Suitable coatings of this type can be prepared from aminoblast polymers, for example reaction products of amines and aldehydes. Typical friable coatings consist, for example, of reaction products of amines selected from urea and melamine with aldehydes selected from formaldehyde, acetaldehyde and glutaraldehyde, and mixtures of said amines and said aldehydes.

Such a friable coating will be described below.

The coated perfume particles of the present invention are useful in situations where the particle coating is ruptured or abraded (eg, in an automatic washer or washer/dryer) to release the particles, which release the perfume. Thus, the coated particles are useful in typical cleaning compositions that include detergent surfactants, optional builders, and the like. Similarly, the particles are useful in conditioning compositions, including fiber and fabric conditioning agents.

All percentages herein are in mi units unless otherwise specified.

DETAILED DESCRIPTION OF THE INVENTION The present invention allows for the preservation, protection and delivery of fragrances contained in cleaning and conditioning compositions through long term storage and harsh cleaning conditions. This is achieved by sequestration of the perfume in the carrier material in the form of small particles. The individual components of the present invention will be explained in detail.

Perfumed Particles The perfumed particles of the present invention consist of a perfume dispersed in a carrier material consisting of. The perfumed particles are coated with a friable coating material, which ruptures during use to release the perfumed particles, and the perfumed particles release the perfume.

In the context of the present invention, the term "perfume" means any substance that gives off a fragrance or acts as a malodor counteractant. Generally, such materials are characterized by a vapor pressure greater than atmospheric pressure at room temperature.

The perfume or deodorant material used herein will most often be a liquid at room temperature, but can also be a solid, such as various camphor-like perfumes known in the art. aldehyde,
A variety of chemicals are known for perfume formulation applications, including substances such as ketones, esters, etc. Exudates consisting of the more common naturally occurring vegetable and animal oils and complex mixtures of various chemical components are known for use as perfumes, and such substances can be used here. The fragrance of the present invention is
The composition can be relatively simple, or it can consist of a highly elaborated complex mixture of natural and synthetic chemical components selected to provide the desired odor.

Typical perfumes of the invention may consist of a woody/earthy base containing exotic substances such as sandalwood oil, civet, bach lily oil, and the like. The perfume of the invention can have a light floral aroma, for example rose extract, violet extract, etc. The fragrances of the present invention have desirable fruity odors, e.g.
It can be formulated to impart odors such as lime, lemon, and orange. Suitable fragrances include musk ambrette, musk ketone, musk ketone, musk quidylol, aurantiol, ethyl vanillin and mixtures thereof.

Fragrance substances, such as S, Arctander, Perfume Flavors End 1 Chemicals (
Perfull Flavors and CheI
Iicals).

Vol.

Procedurally speaking, any chemically compatible material that exudes a pleasant or desirable odor can be used in the perfumed particles of the present invention to impart the desired odor when applied to fabrics.

Perfumes that are normally solids can also be used in the present invention.

Unless the fragrance sublimes or decomposes on heating, these
It may be mixed with a liquefying agent such as a solvent before being incorporated into particles.
Alternatively, it may be melted and blended.

The invention also encompasses the use of materials that act as malodor counteractants. These substances, hereinafter referred to as "fragrances", may not themselves have a discernible odor, but can mask or reduce any unpleasant odor. Examples of suitable malodor counteractants include U.S. Pat.
．． 102. No. 101.

The perfumed particles of the present invention can even include fragrances that are not typically used to deliver fragrance to surfaces such as fabrics through the laundry process.

Flavoring substances that are highly volatile, unstable, or soluble in the particular composition to be used to deliver the fragrance are considered in the present invention because the fragrance is separated from the composition in the particles. May be used. The particles deliver the fragrance to the fabric surface,
Perfume materials that are not substantive to the fabric during the washing process can also be used in the present invention since the perfume is released there. Thus, using the present invention to deliver perfume to a surface expands the variety of perfume materials that can be utilized.

Generally, the perfumed particles of the present invention contain from about 5% to about 70% perfume.
%, preferably from about 5% to about 50%. The exact amount of fragrance used in the particles will vary widely depending on the intensity of the particular fragrance used and the odor effect desired.

The carrier material of the perfumed particles must meet criteria to be useful in the present invention. First, the carrier material must be a water-insoluble polymeric material. Additionally, the carrier material should have a molecular weight of about 100 to about 30,000, preferably about 500 to about 5000. The molecular weight of carrier materials can be determined by any standard method. The carrier material should also have a melting point of about 37°C to about 190°C, typically 37°C to 130°C. This will prevent the particles from melting during storage or in the washer in laundry applications (to avoid clogging of the lint sieve and excessive build-up of heat in the dryer) It is most desirable to have a carrier material that will not melt). Also, the melting point of the carrier material should not be higher than the point at which the perfume to be combined with the carrier material will decompose. The melting point of a homogeneous carrier is determined by what is called the drop melting point method. American Society for Testing End Materials (
ASTM) Test method D127-63 (reapproved in 19B2). Briefly, the method includes the following.

The sample to be measured is deposited onto the thermometer bulb by dipping the chilled thermometer into the molten sample. The thermometer carrying the thermometer is then placed in the test tube and heated by a water bath until the sample melts and a first drop falls from the thermometer bulb. The average temperature at which a droplet of a sample falls is the drop melting point of the sample.

Also, the polymeric material must have a certain hardness. This hardness value may be determined by the standard test method for petroleum wax penetration.

ASTM Test Method D1321-86° Briefly, this method involves first melting and heating the sample to be tested at 17°C below the freezing point.
Includes further heating to a temperature 30°F (°C) higher. The sample is then poured into a container and air cooled under controlled conditions. The sample is then conditioned in a water bath at the test temperature. The penetration is then measured with a penetrometer. This penetrometer applies a standard needle to the sample under a load of 100 g for 5 seconds. The penetration or hardness value is the depth (in tenths) that a standard needle will penetrate into the wax under these specified conditions. The hardness value of the carrier material to be useful in the present invention ranges from about 0.1 to about 15, preferably from 0.1 to about 15.
Must be 8. This would allow particles of hardness that would optimize perfume protection/preservation in the carrier.

The carrier material must also be perfume inert and relatively odorless. The carrier material must allow diffusion of the fragrance therethrough. The carrier material must also be such that it melts without decomposition.

Non-limiting examples of useful carrier materials include those that meet the above criteria and are, for example, water-insoluble and have a molecular weight of about 100 to about 30;
000, with a melting point of about 37°C to 190°C and a hardness value of 0
．． Polyethylene, polyamide, polystyrene, polyisoprene, polycarbonate, polyester, polyacrylate, vinyl polymer and polyurethane having 1 to 15 and mixtures thereof.

Highly preferred supports have hardness values of 0.1 to 8, typically 0. 5. Molecular weight 500-5. 000 (typically 2,000) and a melting point of about 126° C. and would typically be polyethylene.

The 19 carrier materials that meet all of these specified criteria are manufactured by Vetrolite Specialty Polymers Group under the trade name POLYWAX.
It is sold for 2000. This material has a molecular weight of approximately 2.
000, melting point approximately 259″F (126°C) and 77′F
Hardness value at (25℃) (when measured as above) approximately O
85 polyethylene. Another material that fills these Mlls is Polywax 1000 (sold by Petrolite Specialty Polymers Group). This material is also polyethylene with a molecular weight of about 1,000°, a melting point of about 237'F (114°C), and a hardness value at 77"F (25°C) of about 1.0. Another such material is Polywax 500.

It may be desirable to utilize mixtures of different carrier materials, for example blends of polymeric materials and trace amounts of wax materials, in the perfume particles of the present invention. Examples of useful wax materials include the trade name BOLER 1014, Star'
7 t')7. STARWAX 100 and VICTORY (all available from Polar Petroleum Company). Such blends allow for better adhesion since particles prepared from such blends have a "stickier" surface. A large number of combinations of materials are possible and intended to be covered by the present invention, as long as the final blend of carrier materials meets the above criteria.

The choice of carrier material to be used in the perfumed particles of the invention is
The extent to which this occurs will depend on the particular fragrance being used.

Some perfumes will require greater amounts of protection than others, and the carrier material to be used with them can be chosen accordingly.

Generally, the perfumed particles for use in the present invention will contain from 30% to about 95% carrier material, preferably from about 100% to about 95%. Again, this will vary depending on the type and amount of particular fragrance utilized.

In a typical method, perfume-containing particles can be prepared as follows. First, the carrier material is slowly heated to its melting point. The carrier material is heated no more than is necessary to just melt the material.

The perfume is then rapidly added to the molten carrier material, generally as an oil or liquid at room temperature. Mix the two quickly to get a homogeneous blend, then add liquid nitrogen (
or dry ice or other means that will cool the mixture quickly). The solid material is then subdivided, generally by grinding or milling, to prepare particles of the desired average size. Other methods, such as spray cooling or extrusion, may also be used to subdivide the particles.

In order to further stabilize particularly volatile or delicate perfumes, it may be desirable to preload the perfume (ie, mix the perfume) onto the silica gel or clay before combining with the carrier material. Some fragrances that are not very volatile are
Release from the carrier material will be so inhibited that this special treatment will not be necessary. Optimization of the rate of release of perfume from the carrier is the goal and this optional additional step allows better control of rate in some cases of more volatile perfumes.

Coating The perfume-containing particles are encapsulated to provide a friable coating. This coating prevents the perfume from easily diffusing from the particles during long storage periods. Furthermore, the coating helps preserve the original "character" of the perfume, especially with volatile top notes.

Additionally, the coating helps protect the perfumed particles from other ingredients in the formulation to be perfumed.

The coating material used herein is made to be friable and to rupture upon use of the perfumed formulation, thereby releasing the perfumed particles.

The particles may be coated with more than one friable coating material to prepare particles with more than one layer of coating. Different coating materials can be chosen to provide different fragrance protection as desired, so long as the coating 19, generally the outermost layer, is friable.

Individual perfume-containing particles may also be aggregated with a coating material to provide large particles consisting of a large number of individual perfume-containing particles. This aggregate material surrounding the particles provides an additional barrier to diffusion of perfume from the particles. Such an approach also minimizes the surface area of free particles susceptible to perfume diffusion. The ratio of perfume particles to aggregate material will vary widely depending on the degree of additional protection desired. This aggregation approach may be particularly useful in the case of highly volatile perfumes or perfumes that are particularly susceptible to deterioration.

Also, the agglomeration of very small perfume particles will provide additional protection against premature diffusion of perfume.

Agglomeration of particles in this manner is useful, for example, in preventing segregation of small perfume particles from larger detergent granules in dry granular detergent products.

Manufacturing process In the case of friable coatings, the manufacturing process is based on applying the coating as a kind of "shell" to the perfumed particles. In the case of perfumed particles in which the carrier material has a melting point lower than the boiling point of the solvent used in the method, the method involves melting the carrier and perfume together and keeping the molten mixture above the carrier melting temperature. and adding a "shell" material or a suitable precursor to a solvent solution. The system is agitated sufficiently to prepare an emulsion of the desired droplet size of carrier/flavor in the shell solution. The conditions necessary to deposit the encapsulating material are then established and the mass is cooled to create the encapsulated solid particles with the desired friable "shell." The water insolubility of the shell is established during the deposition step or by isolation of the particles or by suitable treatment prior to use.

Although the methodology described herein is a one-step melt droplet formation/encapsulation method, it should be readily apparent to those skilled in the art that encapsulation of pre-6ii2i perfume particles can be accomplished in a similar manner. . Pre-(iii) W particles can be prepared by cryogenic grinding, spray drying, spray congealing and melt dispersion techniques such as P,
A book by B. Daisy ("Microencapsulation and Related Pharmaceutical Methods", Detzker, New York, 1986)
year) and A.

They can be prepared in a variety of ways, including those described in the book by Condo ("Microcapsule Processing and Technology", Detzker, New York, 1979). Such techniques would be required for carrier materials that have a melting point higher than the boiling point of the solvent.

Various suitable encapsulation methods, such as those discussed in the aforementioned two books by Dayley and Condo, include:
Can be used. Depending on the material used, the shell can impart hydrophilic or hydrophobic properties to the particle. Non-limiting examples of encapsulation materials and methods include, in the case of hydrophilic shells, complex coacervation methods, e.g. gelatin-gum arabic concentrates deposited according to U.S. Pat. No. 2,800,457; and polycondensation methods in the case of hydrophobic shells, e.g., U.S. Pat. No. 3,516.94.
Urea-formaldehyde attached by No. 1 Mei IB may be mentioned.

Water insolubility of the shell material may be imparted by crosslinking of the gelatin-gum arabic coacervate with a suitable aldehyde or other known gelatin hardening agent after deposition. Polymerization of the urea-formaldehyde precondensate during the encapsulation process results in water insolubility.

The slurry containing perfume particles can be used directly, eg, spray dried with other ingredients of the formulation, or the particles can be washed, separated and dried if desired.

Example I Perfume particles containing a hydrophilic coating attached by complex coacervation are prepared as follows.

Polywax 500 (molecular weight 5
132 g of polyethylene (polyethylene with 0.00%) are heated at approximately 100° C. in a beaker on a hot plate. 44g of fragrance at room temperature
is added to the molten polywax 500 and heating is maintained to return the core temperature to 100°C.

Add the molten core material to 400 g of a 5% aqueous gelatin solution (Sanafl type A1 bloom strength 275) maintained at a temperature 15-20°C above the melting point of the core in a 1 g stainless steel beaker and add the desired droplet size. Approximately 100μ
Emulsify by stirring until . Next, 200g of hot 11% gum arabic solution was added and stirred for about 30 minutes.
Maintain for minutes.

The pH was lowered to about 4.2 by dropwise addition of glacial acetic acid, then
Pour the beaker contents into stirring water 11 at room temperature. This solidifies the core mixture and concomitantly deposits the gelatin-gum arabic coacurvate.

The coating is solidified by cooling the slurry in ice water to about 5°C. The slurry may be used at this point, or the particles may be separated from unattached coacurvate in the slurry by adding approximately equal volumes of 10% sodium chloride and removing the capsules in a branch funnel. This may be repeated as necessary to completely remove the am niaturbate. The particles are filtered and
The filter cake may be washed with water, then with Inobiopanol, and then dried by air drying at 25° C. overnight.

The particles may then be sieved to the desired size range.

Example ■ Perfume particles with a hydrophilic coating of lower water solubility can be prepared as follows.

A slurry of perfume particles containing a gelatin-gum arabic coating is prepared as in Example I. After cooling, the slurry was warmed to room temperature and 25% glutaraldehyde aqueous solution 8.0
ml under stirring. The pH is raised to 5.0 by the addition of 2.5% aqueous sodium hydroxide and the slurry is stirred overnight.

The slurry may be used at this point or separated as in Example I.

Glutaraldehyde treated coatings can withstand long immersion in water at 60°C, while untreated coatings
It is removed upon heating to 0°C.

Example ■ Perfume particles containing a hydrophobic, water-insoluble coating deposited by polycondensation are prepared as follows.

The urea-formaldehyde ffN condensate was first adjusted to pH 8.0 with 0.53 g of sodium tetraborate.
A mixture of 162 g of % aqueous formaldehyde and 60-65 g of urea was heated at 70° C. for 1 hour, then 2 g of water
Prepare by adding 76.85 g.

Then, 429 ml of this precondensate and 142 ml of water
is stirred in a 1 g stainless steel reactor and 57.14 g of sodium chloride and 0.57 g of sodium carboxymethyl cellulose are added.

Next, 161.3 g of Polywax 500 carrier and 6 fragrances were added.
A core component consisting of 0.7 ml is added and the reactor is heated to about 10° C. above the melting point of the core.

Adjust the agitation to emulsify, maintain the molten core at the desired droplet size, and adjust the pH of the contents to about 5.0 with dilute hydrochloric acid.

The reactor was then allowed to cool to room temperature and the pH was increased over a period of 2 hours.
gradually lower it to 2.2. The reactor is then heated to about 50° C. for a further 2 hours and then, after cooling to room temperature, the pH is adjusted to 7.0 with 10% sodium hydroxide solution.

The slurry containing solid core particles encapsulated with urea-formaldehyde polymer may be used directly or may be subjected to separation, washing, and optionally air drying.

The coated perfumed particles prepared by the above method can be used in all types of products where it is desirable to deposit a fragrance onto a treated surface and where sufficient agitation or pressure is applied to break the friable coating. Typical examples of such products that can be used are laundry detergents and fabric softeners. The following illustrates the use of compositions of the invention in such products.

Laundry cleaning products typically contain detergent surfactants; usually one or more detergent builders; optionally various enzymes, bleaching agents,
carriers, etc. (all well known from standard textbooks and very familiar to detergent formulators). Surfactants include soaps, alkylbenzene sulfonates, ethoxylated alcohols, alkyl sulfates, and the like.

As builders, various phosphates, zeolites,
Examples include polycarboxylate.

U.S. Patent No. 3,985,669, No. 4°379
．． No. 080 and No. 4,605.609 may be referenced for exemplary lists of such ingredients.

Modern fabric softeners typically contain one or more quaternary ammonium salts, or imidacillin or imidazolinium compounds. Softeners (and antistatic agents) generally have one or preferably two 012-018 alkyl substituents and two or three short chain alkyl groups. Again, such materials are common and well known to fabric softener formulators.

Example ■ Granular laundry detergents are as follows.

component Sodium C13 alkylbenzene sulfonate thorium Sodium C alkyl sulfate 14-15 Unnidoxylated alcohols and lower removed ethoxylate C Alkylboriethoxyle 12~(3 Oneto (6,5) C12 alkyltrimethylammonium Muchloride Sodium tripolyphosphate sodium carbonate Sodium perborate monohydrate Octanoyloxybenzene sulfo Sodium phosphate Sodium diethylenetriaminepentaacetate Umu Sodium sulfate, H20, minor components weight% 1.0 32.0 10.0 43 remainder The compositions are prepared using conventional means.

The composition is combined with the perfume particles of Example 1 as follows.

The detergent composition has a fragrance level of 0. A predetermined amount of perfume particles of Example I is combined with a detergent composition to contain 3%.

The particles may simply be mixed with detergent granules.

To prevent segregation of the fragrance particles during packaging and transport (due to the smaller size of the particles compared to the detergent granules), the particles are optionally coated with a water-soluble coating substance before combination with the detergent granules. Can be coated or aggregated (on top of friable coating). This means that the Schugl mixer [Flexomix (PI (3XOIIX) 16
0), in which a sufficient amount of dextrin adhesive solution (2% dextrin, 3% water) is sprayed onto the particles to form agglomerates of perfume particles within the same size range as other detergent granules. arise.

The fragrance is protected in the particles from deterioration by bleaching agents in detergent compositions over long shelf life. When used in a laundry process in an automatic washing machine, the detergent composition will impart a substantially intact perfume aroma from the product onto the fabric through the cleaning process.

A large number of fragrances can be utilized in the present compositions that would otherwise not be suitable for use in laundry detergent compositions.

Example V A liquid fabric softener for use in an aqueous laundry rinse bath is as follows.

component Softener A★ Softener B*” weight% 3.00 5.00 0.29 0.15 0.30 00ppm 0ppm 30ppa+ 4.0 remainder C.I. polydimethylsiloxane Polyethylene glycol (4000) Pronopol (antibacterial agent) calcium chloride dye Coated fragrance particles **” water ★Softener A is the formula (In the formula, each R2& is within the C15-C18 alkyl range) has.

*”Softener B is the formula (In the formula, each R group is within the C15-C18 alkyl range) has.

★★★ Particles prepared according to Example ■.

size 100μ; coating type ff15%.

When used in the rinse bath of an automatic washing machine, the coating on the perfumed particles of Example V is broken and the particles impart fragrance to the fabric to be treated.

Example■ The liquid laundry detergent composition is as follows.

Component CI3 Linear alkylbenzene sulfonic acid C14-15 alkyl polyethoxylate (2,25) Sulfuric acid C alcohol polyethoxylate (6,5)★12-13 C12 alkyltrimethylammonium chloride Ci2
~l-fatty acids oleic acid citric acid (anhydrous) diethylenetriaminepentaacetic acid protease enzyme (2, OAU/g) amylase enzyme (375 Am, U/g) ★★ TEPA-E15-18 Monoethanolamine (moles of alkanolamine) Sodium ion weight% 7.2 IO18 B, 5 1.2 13.0 2.0 4.0 0.23 0.75 0.1B 1.5 2.0 (0,033) l, 66 Potassium ion
2.65 (molar ratio of K:Na)
(0,94)propylene glycol 6,
8 ethanol
7.8 formic acid
0.8B calcium ion 0.
03 Trace components and water Remainder (assumed to be 100) Concentration in water at 68°F (20°C) 10
% pH 8,65★Alcohol and monoethoxylated alcohol removed.

★★15 to 18 moles of ethylene oxide at each hydrogen site (
The ethoxylated tetraethylene pentimemine detergent is prepared by adding the ingredients under continuous mixing in the following order: Paste premix of alkylbenzene sulfonic acid, sodium hydroxide, propylene glycol and ethanol: alkyl poly Paste premix of dipentaacetic acid with ethoxylate sulfuric acid, sodium hydroxide and ethanol; alcohol polyethoxylate; premix of water and brightener with alkanolamine and alcohol polyethoxylate; ethanol; sodium hydroxide and potassium hydroxide; fatty acids; citric acid; formic acid and calcium; alkyltrimethylammonium chloride; TEPA-E, 5-18; regulating the pH to about 8.1; and the remainder of the ingredients.

The above composition is combined with the perfume-containing particles prepared according to Example 1 as follows. A predetermined amount of perfume particles (average size range 40 to
150μ; 5% coating) is thoroughly incorporated into the liquid detergent composition (approximately 1% of the detergent composition will consist of perfume particles).

Example■ Fiber and fabric softener compositions include: Ru.

component Softener C* TAMET★★ GMS★★★ phosphoric acid weight% 3.7 0.3 engineering, 20 0.023 It is as follows (350) 0.10 50ppm 10pp bias 3.0 Br　　C In the formula, (i.e. “Taro polydimethylsiloxane glutaraldehyde blue dye Coated fragrance particles*** ★(R1)2(CH3)2N + R1 is mixed c-c alkyl 12 18 alkyl)].

★★TAMET is Tallowalkyl N (CHCHOH) 2.

　　　2 ★★★GMS is glyceryl monostearate.

★★★★Coated fragrance particles according to example (■) sieved to an average size of less than 150μ. Coating weight 3%.

It is noted that the anion, X, used in any of the cationic fabric softeners of the present invention is a matter of customary choice, and that X can be, for example, chloride, promide, methyl sulfate, etc. will be recognized by those skilled in the art. Mixtures of fabric softeners can be used, as can mixtures of anions.

Example ■ The detergent composition of Example ■ was 1% and 2% by weight of the coating, respectively.
Friable coating with 0% (melamine/urea/formaldehyde; molar ratio 0.1/1/1.1; size 300
amended by using perfumed particles with μ).

Example ■ A detergent solid composition is prepared using the coated perfumed particles of Example I (coated 7
%; all particles pass through a 150 μ sieve) 2% by weight to 9
Prepared by gently incorporating into a 9.44% tallow soap mixture (Na salt) (so as not to break the coating) and forming into a solid in a binder die.

This composition can also be used in combination with an abrasive.

As is well known, abrasive cleaners typically contain 10% to 90+ abrasives such as pumice, silica, calcium carbonate, etc.
%including. The coated perfume particles used in such cleaners rupture during use, releasing the perfume.

Example X Abrasive cleaners are as follows.

Ingredients Weight% sodium tallow sulfate l, 0 calcium carbonate
40.0 pumice (passed through a 60μ sieve)
45.0 Sodium sulfate
10.0 Coated fragrance particles *3.0 Chlorinated trisodium phosphate 1.0★Example■
Compliant with; coating 10%; particles passed through a 100μ sieve.

The composition of Example X is prepared by gentle dry blending the ingredients.

It will be appreciated by the formulator that the weight (or thickness) of the usable friable coating can be adjusted according to the intended use. For example, even relatively thick coatings will rupture and release perfume particles under European machine washing conditions, which can include high temperatures, considerable agitation and many minutes of washing time. In contrast, US machine cleaning conditions are much shorter and milder, and therefore less coating material should be used. For fabric softeners, agitation and agitation times are typically less than for washing.

Claims (1)

[Scope of Claims] 1. Coated perfume particles having an average size of about 350μ or less when coated, a molecular weight of about 100 to about 30,000, a melting point of about 37°C to about 190°C, and a hardness value of about 0.1 to about Approximately 15
from about 5% to about 70% of a perfume dispersed in about 30% to about 95% of a water-insoluble polymeric carrier material having a composition, said particles having a friable coating on their outer surface. Coated perfume particles. 2. Particles according to claim 1, having an average size of 150μ or less. 3. Particles according to claim 2, which are within the size range of 40 to 150 microns. 4. Particles according to claim 1, wherein the coating constitutes up to 20% by weight of the perfumed particles. 5. Particles according to claim 4, wherein the coating constitutes 1-10% by weight of the perfumed particles. 6. Claim 1, wherein the friable coating is substantially water-insoluble.
Particles described in. 7. Particles according to claim 6, wherein the coating consists of an aminoblast polymer. 8. Particles according to claim 7, wherein the coating consists of a reaction product of an amine and an aldehyde. 9. The particles according to claim 8, wherein the coating consists of a reaction product of an amine selected from urea and melamine and an aldehyde selected from formaldehyde, acetaldehyde and glutaraldehyde, and a mixture of the amines and the aldehydes. . 10. The particle of claim 1, wherein the carrier material has a molecular weight of about 500 to about 5,000 and a hardness value of about 0.1 to about 8. 11. Particles according to claim 10, wherein the carrier material is selected from the group consisting of polyethylene, polyamide, polystyrene, polyisoprene, polycarbonate, polyester, polyacrylate, vinyl polymer, polyurethane, and mixtures thereof. 12. The carrier material has a molecular weight of about 2,000 and a melting point of about 126.
10. Particles according to claim 9, consisting of polyethylene having a hardness value of about 0.5. 13. A detergent composition comprising one or more detergent surfactants, optionally one or more builders, and perfume particles,
a water-insoluble polymeric carrier material having a molecular weight of about 100 to about 30,000, a melting point of about 37°C to about 190°C, and a hardness value of about 0.1 to about 15;
from about 5% to about 70% perfume dispersed from 0% to about 95%, the particles having a friable coating on their outer surface;
A detergent composition wherein the coated particles have an average size of about 350 microns or less. 14. The average size of the coated particles is 150μ or less,
A composition according to claim 13. 15. The friable coating is an aminoblast polymer.
A composition according to claim 14. 16. The composition according to claim 15, wherein the coating is a reaction product of an amine selected from urea and melamine or mixtures thereof, and the aldehyde is selected from formaldehyde, acetaldehyde, glutaraldehyde, or mixtures thereof. 17. The composition of claim 16, wherein the coating constitutes 1-10% by weight of the particles. 18. The composition of claim 13, wherein the carrier material has a molecular weight of about 500 to about 5,000 and a hardness value of about 0.1 to about 8. 19. The composition of claim 13, wherein the carrier material is selected from the group consisting of polyethylene, polyamide, polystyrene, polyisoprene, polycarbonate, polyester, polyacrylate, vinyl polymer, polyurethane, and mixtures thereof. 20. The carrier material has a molecular weight of about 2,000 and a melting point of about 126.
17. The composition of claim 16, consisting of polyethylene having a hardness value of about 0.5. 21. The composition of claim 13 in solid form. 22. The composition of claim 13, additionally comprising an abrasive. 23. A softener composition comprising one or more fabric or fiber softeners or antistatic agents and perfume particles, having a molecular weight of about 100 to about 30,000 and a melting point of about 37°C to about 190°C.
and about 5% to about 5% perfume dispersed in about 30% to about 95% water-insoluble polymeric carrier material having a hardness value of about 0.1 to about 15.
70%, the particles have a friable coating on their outer surfaces, and the coated particles have an average size of about 350 microns or less. 24. The average size of the coated particles is 150μ or less,
A composition according to claim 23. 25. The friable coating is an aminoblast polymer;
A composition according to claim 23. 26. The composition of claim 25, wherein the coating is a reaction product of an amine selected from urea and melamine or mixtures thereof, and the aldehyde is selected from formaldehyde, acetaldehyde, glutaraldehyde, or mixtures thereof. 27. The composition of claim 26, wherein the coating constitutes 1-10% by weight of the particles. 28. The composition of claim 23, wherein the carrier material has a molecular weight of about 500 to about 5,000 and a hardness value of about 0.1 to about 8. 29. The composition of claim 23, wherein the carrier material is selected from the group consisting of polyethylene, polyamide, polystyrene, polyisoprene, polycarbonate, polyester, polyacrylate, vinyl polymer, polyurethane, and mixtures thereof. 30, the carrier material has a molecular weight of about 2,000 and a melting point of about 126
27. The composition of claim 26, consisting of polyethylene having a hardness value of about 0.5.