CA1285153C - Method for foliage and other plant material preservation and topical color application to same - Google Patents

Method for foliage and other plant material preservation and topical color application to same

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Publication number
CA1285153C
CA1285153C CA 533063 CA533063A CA1285153C CA 1285153 C CA1285153 C CA 1285153C CA 533063 CA533063 CA 533063 CA 533063 A CA533063 A CA 533063A CA 1285153 C CA1285153 C CA 1285153C
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Prior art keywords
plant materials
ethylene glycol
materials
treated
plant
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CA 533063
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French (fr)
Inventor
Jeffrey Lee Dokkestul
Leo Arthur Ochrymowycz
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Individual
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Individual
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Priority claimed from US06/889,253 external-priority patent/US4664956A/en
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Abstract

METHOD FOR FOLIAGE AND OTHER PLANT MATERIAL PRESERVATION
AND TOPICAL COLOR APPLICATION TO SAME
ABSTRACT
A method for preserving natural plant material comprising immersion, under about 3 to 30 psig (0.21-2.1 kg/cm2 gauge) pressure, the material in ethylene glycol having a specific gravity of 1.03 - 1.10 for a period of four hours to five days. The material is then withdrawn, washed and dried for use or further treatment. The spent ethylene glycol is restored to its original volume with virgin ethylene glycol and re-used many times without purification. The preserved plant material is topically coated with an hydrophilic polymeric sealer optionally blended with a pigment.

Description

METHOD FOR FOLIAGE AND OT_~ER PLANT MATERIAL
PRESERVATION AND TOPICA. COLOR
APPLICATION TO .SAME

Bac]cqround of the Illvention 1.Field o~ the Invent~on This invention rela-tes to preservat:ion o~
Poliaye or l.;ke materials derived from ~reshly harves-ted plan-ts, eithe.r under cultivation or from indigenous wild sources, by pressure injection with a humectant. Such materials are intended for decorative utilization, to be ofEered for sale through the Eloral trades industry.
2. Information Disclosure Statement The preservation and rendering natural in appearance of various plant materials for decorative, scientific, or display purposes of an aesthetic nature have been previously described in a variety of U.S.
patents. Various parallel but unli]ce claims have been offered in other U.S. patents. Bridgeman et al U.S.
Patent No. 2,057,413 describes a process for preserving living plants, cuttings, roots, bulbs and the like by coating with an aqueous emulsion of carnauba wax and an oleic acid salt.
In Dux U.S. Patent No. 2,026,~73, ruscus, lready bleaahed and dyed, is softened by soaking 2-5 ~ ', ~

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5~ 3 minutes in an emulsion of ylycerin and sulphonated vegetable oil.
Dux U.S. Patent No. 2,083,191 discloses a method for bleaching and/or dyeing foliage by submerglny in ethyl or methyl alcohol at e.levated pressure and temperature. The alcohol can be used only for 4-6 batches because wa-ter displaced from the oliaye dilutes the alcohol to below 172 prooE, too low for proper bleachiny. This is true despite replenishment of alchohol ahsorbed by the foliage.
l~orupp et al IJ.S. Patent No. 1,484,656 describes a process for producing decoratlve oliage. Cut plants are first dried, and then softened in a a~ueous mixture of ylycerin and formalin. After the plant surfaces are again dried, paint and/or varnish is applied to seal the glycerin within the treated plant.
Complete pre-drying is essential to adhesion o the paint or varnish to the foliage.
In Romero-Sierra et al U.S. Patent No's.
4,278,7~5 and 4,328,256, plant tissues are preserved with their natural color fixed by immersion in a complex solution containing (a) water, (b) an alchohol exchange medium, (c) preservatives, and (d) buffers, mordants and modifiers.
Sheldon et al U.S. Patent 3,895,140 describes a process for preserving cut green foliage by extracting the normal fluidr therefrom and imbioing a polyol, ....
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~ 3~..5`3 e.g. glycerin, in place thereof, at 140-250F. The preserved foliage may be dyed by soaking in pigment containing glycerin solutions.
It has been set forth in U.S. Patent No.
4,287,222 to Robinson that fresh foliage material or other plant materials of a slightly dehydrated nature can be preserved by the injection under pressure o~
humectants belonging to the polyol class o~ materials, suah as glycerin, ethylene glycol, and various polyethylene glycols. Most specifically, its claims demand that the density of such humectant material should fall within the speciEic gravity range of 1.10 and 1.16. Commensurate with such preservation ; techniques is the coloring of such materials by the direct combination of compatible dyes with the humectant agent, which are likewise forced under pressure in the plant materials. Subsequently, after apporopriate duration of treatment with both humectant and dye, the plant material is withdrawn, rinsed in cold water, and dried to a natural state. It has been our experience, in fact, in evaluating the Robinson claims that no dye, out of fourteen classes of dyes involving at least one hundred combinations of dye materials, retained the desired stay-fastness in the plant foliage. In our tests, the specific dyes cited in the patent failed to achieve the desired result.
Moreover, with the exception of the basic green-l ' .
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class of dyes, none of the dyes was unlformly absorbed in-to the material so as to render a natural color. No dye likewise was found which provided in the end result a stay-fastness of any signiEicant duration.
Finally, under no circumstances were we able to demonstrate consistency in preservation which resulted in the desired natural conEiguration, teix-ture and structural retention of foliage with any combin~-tion of glycerol water. At glycerol concentrations specified in the Robinson patent, and even at concentrations as low ais those with a specific gravity of 1.08, extensive swelling and rupture of the plant tissue cells was observed by frozen section microscopic analysis. The ylycerol humec-tant subsequently escaped the foliage structure by evaporation and biodegradation. The so-called preserved foliage rapidly curled, dried and decomposed.

SUMMARY OF THE INVENTION
In developing alternative methods, we have observed that numerous mitigating factors contribute to the behavior of natural plant material, including foliage, under humectant pressure treatment. These include the freshness and development stage of foliage, the type of foliage to be utilized and most critical for uniform large scale preparation of ' ' .

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preserved materials, the nature o~ the humectant.
Accordingly, a present objective of this invention is a method for treating freshly harvested plant materials, specifically foliage materials, which does not entail any prior process of denaturing such foliage materials by bleaching, the addition of chemica.l additives, or any process other than optional cleaning of the foliage by simple water-surEactant wash prior to its preservation. Even such washing may be omitted i~ the foliage is free of any surface contaminants. The objective is to yield as an end result a material that has long term shelf life and long term use for decorative or ornamental purposes, as well as educational, expositional, and sentimental purposes. More specifically, an objective is to produce a treated and coated material which has a minimum shelf life of six months at 60-90F (16-32C) and 50 percent relative humidity. More preferably, a shelf life of at least one year is desired. Because the prime harvest season is : relalatively short, foliage is generally treated for preservation and stored for later color application.
Thus, the treated but unsealed and/or uncolored material will preferably have a shelf life of at lea~t ;25 four months. However, the scope of the method does not require that the terminal appearance of the ~.

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, 5~ ~3 foliage is to be absolutely natural and lifelike, although the process described within will in fact meet such qualifications. lt is possible by the present invention to generate foliage having virtually any color, whether natural or exotic in nature, dependent only on availability of the requisite colored coating formula-tion. Thus, foliage of numerous colors, as well as foliage having a colorless appearance, can be formulated and prepared to have the configuration of living foliage. The terminal objective of the present invention is to in fact provide a process at a high level of performance conducive to large scale manufacturing production of said materials. Whereas the mere preservation of the foliage material may not involve a specific dexterity related to artistic considerations, the coloration of the material by application of surface coatings and its texturing to natural color does involve the aesthetic judgment of artistic color texturing.
However, the materials involved in application of such artistic texturing are formulations of commercially available materials designed to achieve specific aesthetic effects.
In summary, this invention is a method for preserving natural plant materials, including cut foliage, to enhance their appearance and decorative ~ . .. .. .... .

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A batch of the plant materials is ~irst immersed in a starting volume of ethylene glycol having a specific yravity of 1. 0~ to 1.10 at a pressure oE
about ~ - 30 psig (~bout 0. 21 - 2 .1 kg/cm2 gauge) for a period o~ four hours to five d~y~ Thi~ range of specific gravity corra~ponds approximately to 2~-77 percent ethylene glycol. The plant Eluids are partially exchany~d wi~h ethyl~n~ glycol, producing treated plant materlals containing ethylene ylycol of specific gravity 1.025 - ~.10. The lower value of speci~ic gravity, i.e. 1.025, corresponds to approximately 19 percent ethylene glvcol.
The treate~d materials are withdrawn from the pressurized immersion in the spent ethylene glycol and washed to remove excess ethylene y]ycol from their surface. The materials are then drled to the touch for use or further treatment.
The spent ethylene glycol is restored to its starting volume by adding ethylene glycol having a concentration no lower than specific gravity 1.03.
PreEerably, virgin ethylene glycol is used. The restored humectant is reused to treat additional batches of plant materials according to this process.
The use of fungicides, bactericides, dyes, buffers, moxdants, and/or modifiers in the exchange , , :

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Following treatment with ethylene glycol, the plant materials may be topica:Lly coated by one of several methods.
In one method, the maeria;Ls are first dipped in a hydrophilic polymeric subcoating sealer. The sealed materials may then be topically tinted, if desired, by dip-coating or spraying with a blend of pigment in a water dispersible adhesive or polymeric medium.
Alternatively, the foliage materials may be sealed and tinte~ in a single step, for example with a blend o~ hydrophilic polymer and pigment.

i DESCRIPTION OF THE PREFERRED EMBODIMENTS

1. Preserva-tion and Permanency Retention of I -Folia~e Structure This invention comprises a method which demands as an essential consideration the utilization o~
ethylene glycol in the specific gravity range from 1.10 to as low as 1.03. No other humectant composition has been found to be suitable to meet the same quality of product as that to be obtained from ;~t ethylene glycol. The best results are obtained in a specific gravity range of 1~05 - 1.10, but operational product can be obtained for material of a specific t~
gravity down to as low as 1.03. Optimum results, '' '' I
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however, are ob-tained for the above specific gravity ranye of 1.05 to 1.10, as measured at 20C. The exemplary preservation then involves the bundling of freshly cut foliage which has not been precoated in any way by any agent. Most specifically, prohibition is demanded against the utilization of any other chemical agents, such as fungicides or interim preservatives often utilized to coat foliage. Such materials should all be excluded from material to be utilized for preservation. It is often advantageous to remove any surEace contamination of foreign matter, e.g. dust or dirt adhering to said foliage by a brief washing with cold wa-ter, with or without detergent~
At the same time, however, certain foliages which have been desiccated to a considerable degree may likewise be preserved, as long as their structural integrity was retained following desiccation. Thus, up to about three pounds of all such foliage per gallon of ethylene glycol (0.36 kg per liter ethylene ylycol) are inserted into a large immersion pressure vessel and ethylene glycol is subsequently added to the same vessel. Alternatively, the humectant is placed in the vessel first.
To the ethylene glycol may be added an antifoaming agent in order to suppress foaming or gas entrainment during the pumping of ethylene ~lycol . , :

preservative~humectant in a continuous operation process. Antifoam agents having a silicone base are preferred, although other types may also be satisfactory. The antifoam agent of choice is a silicone defoamer marlufactured by Dow-Corning Company of Midland, Michigan. The specific serial yrade and product line is Anti-Foam DB-llOOA. For two hundred gallons (750 liters) o~ ethylene ylycol, approximately thre.e ounces (85 grams) of the foaming agent is added.
This need not be recharged except after ex-tensive reuti].ization of the ethylene glycol so as to preserve foam suppressions. In one embodiment, the immersion vessel containing ethylene glycol and fresh foliage is then sealed and external pressure of air or other insert gas is applied.
While this method is satisfactory for some materials, most foliage species are more uniformly treated in a shorter time period by expressly eliminating gas from the pressure tanX. In the absence of vigorous agitation, gas bubbles adhere to foliage surfaces and prevent penetration of humectant into the foliage.
Therefore, in the preferred embodiment, the humectants are introduced with a strong flow from the bottom of the vessel to wash out all traces of gases clinging to the foliage surfaces and the gases ~' ;
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entrained in the humectant. ~s the liquid flow is continued and essentially all gas bubbles are purged from the pressure vessel, the outflow at the top of the vessel is closed and hydrostatic pumping of humectant is continued until the desired internal pressure is achieved. Other methods of pressuriziny the vessel may alternatively be used, provided no gas is introduced into the vessel, and the foliage is treated in humectant essentially free of gases. We 10 have observed that for many species, elimination of yas bubbles enables the production of a high quality, uniformly preserved material in a much shorter time.
For most product lines, good penetration and preservation with ethylene glycol is thus achieved in 15 treatment periods as short as four hours. More woody foliage and foliage having a dense structure or massive texture may require longer periods of pressure soaking (eight to twelve hours being typical).
In addition, the elimination of entrained gas by 20 this method also reduces the ef~ects of foliaye maturity and post-harvest age upon the required treatment time. Thus, a uniform~ relatively brief treatment period may be used to ~reat a wide variety of materials without regard to such factors as 25 maturity or post-harvest age.
From a commercial standpoint~ it is advantageous ~5~53 to minimize the processing time without sacrificing quality. We have found that, depending on the particular plant material and operation temperature, an immersion pressure of 3 - 30 psig (0.21 - 2.1 kg/cm2 gauge pressure) produces the best results in a short processing time and at the lowest cost.
The rake of absorption of the humectant and curing of the foliage is directly proportional -to freshness of Eoliage, temperature oE ethylene ylycol, and incrementally related to pressure. The specific pressure ranye is not critical per se. a minimum, however, of approximately 3 psig (0.21 kg/cm2 gauge) to a maximum of approximately 30 psig (2.1 kg/cm2 gauge) produces sakisfactory results. In fact, the preservation and the humectant absorption of the foliage may be done entirely without pressure, but requires considerably longer duration for absorption of the humectant. The optimum temperature range is from 70F (21C) to approximately 105nF (41C), and the best results are achieved with the freshest foliage. Light leaf foliages are readily preserved under such treatment for a period of 4-48 hours.
~eavier wooded foliages, such as leather leaf fern, require a minimum of 48 hours of such pressure treatment. Heavy wooded foliages, leather leaf fern being a good example, and other examples such as .

~3 heather or palms of various lcinds, may in fact be improved in quality of natural characteristic by subsequently withdrawing from the pressuxe treatment process and soaking for an additional period of up to one week at atmospheric pressure in ethylene glycol of specific gravity 1.05 or higher. Preferably, ethylene glycol of specific gravity between 1.07 and 1.10 ls used. During the pressure treatment, and durlng atmospheric coaking, the bulk materials are preferably periodically or continuously ayitated in order to expel any adhering or entrained air-gas bubbles from the foliage matrix. This may be done, for example, by tipping, turning, or rolling the immersion tank to achieve liquid movement through the foliage.
It is most convenient to withdraw the ethylene glycol in large quantity from the pressure tank by an efficient surge pump. The antifoam agent will suppress all foaming during transfer. Likewise, loading of such tanks is best achieved with a high volume surge pump. During such pressure treatment with ethylene glycol, most o the green coloration of chlorophyll is lost from the foliage structure and the ~oliage assumes an off-gray to a grayish-tan coloration.
Freshly withdrawn foliage is stacked in piles on racks from which excess ethylene glycol is drained .

~ 3 into a catch tank. Su~sequently, the foliage is washed with cold water to which has been added only a very small amount of a nonionic deteryent of any variety, or a blended surfactant such as castile soap, e.g. Lux'U soap. Once surface adhesion of ethylene glycol has been removed, the foliaye is shaken free of excess wetting due to water and hung to air dry to a state equivalent to that of natural nonwetted foliage.
The required time for ~rying is inversely proportional to the velocity of air movement within the racked foliage. The drying time may be reduced by increasiny air circulation through the hung foliage and/or by a slight elevation of temperature. Heavily structured foliage, such as leather leaf fern or various palms, may on occasion require a second washing due to a depressurizing blead-out of the humectant ethylene glycol from the material. Subsequent topical coloration of the preserved foliage demands that the bulk of ethylene glycol be cleaned from the foliaye surface. Therefore, the number of washings required to bring the foliage to a surface clean condition varies. Excessive surface ethylene glycol is readily apparent by appearance and feel. Strictly speaking, the dried foliage surface is not free of ethylene glycol. In all cases, a very thin layer of humectant remains at the foliage surface because oE capillary '.' ' ' .

~Z85~;3 action.
Despite dilution ~lith plant moisture, the ethylene glycol recovered from the preservation process may be reutili~ed in effect indefin~tely without any apparent degracla-tion. The only requirement is that additional ethylene glycol having a specific gravi.ty no lower than 1.03 must be added back to the used ethylene glycol to bring the total volume baclc to the starting quantities. PrePerably, virgin ethylene glycol is used. We have observed reutilization of a crude batch of ethylene glycol by the incremental readdition of virgin ethylene glycol for over eighty consecutive preservation runs without loss in product quality. Thus, purification of the ethylene glycol, e.g. by distillation is rarely if ever required. Depending on foliage, anywhere from five to fifteen percent of the original ethylene glycol is taken up from a bath-volume ra-tio of three pounds foliage per gallon (0.36 kg per liter). During such reuse of the ethylene glycol, its specific gravit~ rpaidly falls from the initial starting value of 1.10 to incremental values significantly below l.lo for example, to 1.07 or 1.0~, or even 1.03.
For some foliage lines it is often advantageous to allow the material to cure for one wee~ to two weeks prior to its subsequent utilization. ~lowever, '- , .

: L2~35~53 light grained foliage such as sprengeri or plumosus dry quickly and leave very little residual humectant and may be carried on to the coloration step almost immediately.
In the event that foliage need not be colored for its end use, it may be utilized in its preserved form in a tannish-gray appearance. It slowly changes over a period of four to five days Erom a tan gray to an amber brown color. If exposed to sunlight for varying durations, e.g., 20-100 hours the colvration bleaches to a pale buckskin tan. It is the intent of this invention to market such tan colored foliaye under the color lahel of "Buckskin." Most foliages so exposed to sunlight achieve the "Buckskin" colora-tion within a period of four to five days for an eight hour day of direct sunlight exposure.
The plant material which may be processed by the above invention is most extensive and includes, but is not specifically limited to the following. However, for commercial purposes, the following bear specific note: sprengeri, plumosus, tree fern, ming, plumosus stringers, marsh grass and peopper grass are preserved in two days preservation time. Deer foot moss, Spanish moss, reindeer moss, and other such mosses are preserved in one day preservation time. Various ferns, including leather leaf fern, sword fern, ~ ~ ' ' . ' ' ' .
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~5~53 ~lorida flat fern, and all other such ferns, are preserved in two to three days, followed by optimal results obtained from an additlonal week of soakiny in ethylene glycol at atmospheric pressure. Maynolia and Palmetto likewise require the same treatmenk as leather leaf fern. Sparkle berry, aspidistra, Florida huckleberry, and any other variety of huckleberries;
ivies of all types, including large ivy, grape ivy, small ivy, and ivie~ relat~sd to the mistletoe varieties, can be treated in three days without additional soaking at atmospheric pressure. Florida ruscus, coon tie fern, West Coast huckleberry, West Coast Salal, bear grass, tipi fern, champas, cypress, small Florida bamboo, medium bamboo and large bamboo require three days preservation time without additional soaking. All varieties of pines, spruces and first, including Frasier fir, ~ustrian pine, Florida shortleaf pine, white pine, black spruce, Hamilton spruce, two hemlocks, and all other evergreens, require three days of treatmen-t. The preceding is but a partial list of plant materials which have been processed successfully through the utilization of the present invention. Other foliages are amenable to the same process as described or with only minor variations. The treatment time may vary, depending on the production schedule and plant foliage quality.
z. Application of Lifelike Natural Green Coloran_ and Other Colorants The desirable color and hue may be applied to the preserved plant material by topical-dip application oE an acrylic base subcoating, ~ollowed by a tinting applied under pressure spraying.
Alternatively, a one-step topical coating may be applied, saving time and expene~e. A wide variety of colors and hues may be applied without restriction to the nature of foliage. The critical faator in the two step process is tha-t an appropriate underlayment is first applied to the foliage followed by a very light tinting to bring the foliage to the desired hue. In the case of green or natural appearance the formulation is subsequently described. ~or purposes of example, alternate colorations will likewise be ; described. The practice in general follows in such fashion: The plant material, such as a single leaf or multiple bunches of sprigs, having previously been washed of all surface hemectant, is air dryed, generally above 70F (21C), to the touch. This material is dipped into an hydrophilic base coating which totally masks any underlaying color of the foliage and adheres to the foliage surface despite the layer of ethylene glycol. During the preservation process, the natural chlorophyll green color of the :.

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~8~;~S3 ~oliaye has been destroyed due to dehydration, chemical degradation, or photo fading. Once the base coating has been dip applied and dried, the primary color tonent is applied under pressure spray. The critical feature to be achieved is a coating o~ high integrity, high retentiveness t no tackiness, and luster or texture comparable to natural foliage. IE
alternate~ shades, colors, or hues are re~uire~, these may be achieved without intent to duplicate or simulate natural appearanae.
The following is an exemplary ~ormulatlon for a natural chartreuse green foliage blend. The ~irst to be described is the base coating which is applied by dip to the foliage material. This does not exclude numerous other possible combinations which may result in satisfactory product quality. The base coating achieves its ~ilming and sealing properties from an acrylic-glue blend underlayment. The acrylic underlayment utilized within the exemplary process is manufactured by McWorter Chemical Corporation, Carpentersville, Illinois, and marketed under the trade name oE Aquo-~ac~ 607 or 609 series. Likewise, the exemplary pigments utilizad for the application of appropriate colorants are marketed by Val-Spar Manufacturing, Rockville, Illinois, and marketed under the Tint-EZE~ label. Desired green color combinations are obtained ~rom the four component listing of constituents. These include: Pthalogreen-623, Organic Yellow-611, Titanium White-600, and Lamp Black-691.
In the suhsequent tinting process the base media can be any variety of water dispersable adhesive or polymeric media which binds well to the acrylic underlayment and like the base coat imparts sealant properties upon the foliage. In our proce6s optimal results have been obtained wlth one oE two alternative materials. These include a formalclehyde based adhesive manuEactured by H. B. F'uller Company of Minneapolis, Minnesota, Adheisve X-3801; or alternatively, an antitranspirant manufactured by Agro-K Corporation of Minneapolis, Minnesota, mar]ceted under the label of Envy-Antitranspirant~ The preparation of stock solutions o~ base colorants and tinting agent involve the following:
A. Base Coating Colorant Combination - Green.
Four cups (0.95 liter) of the Pthalogreen-623, two cups (0.47 liter) of Organic Yellow-611, and one cup (0.24 liter) of Titanium White-600, are blended with seven cups (1.656 liter) of water to form a dispersed paste. To this dispersed paste is mixed two gallons (7.57 liters) of the Aquo-Mac~ 607 or 609.

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~S~3 B. Stock Solution Base Colorant - Yellow.
Five cups (1.18 liters) of Oryanic Yellow-611 is likewise blended with five cups (1.18 liters) of water to produce a dispersant-paste. This is likewise blended with two gallons (7.57 liters) of Aquo-Mac'~
607 or 609. Usiny the above stock blends, the mixture designed as the dipping coat is then formulated as Pc~llows: Seven quarts (1.656 liters) of the green piyment stock, _, are mixed with six quarts (1.42 liters) of the yellow piyment stock, B, and added to two gallons (7.57 liters) of 50:50 aqueous Adhesive 3081, or two yallon~ (7.57 liters) of 50:50 a~ueous Envy-Antitranspirant~. After efficient blending the total mixture is then diluted with twenty gallons ~75.7 liters) of methyl alcohol. This then constitutes the base dip material. In the event that foliage is being utilized which is very nonuniform in color due to the preservation process, or due to bleach out of background colorants due to the preservation process or sun exposure, trace amounts of Lamp Black-691 are then blended to obtain depth of tone.
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On most occasions, no Lamp Black need be added. The amounts wh:ich are added in exceptional cases constitute quantities in the vicinity of a tablespoon (15 mL) or less. If a heavier application of coating in the base coating dip process i8 desired, then lesser ~uantities of methanol are utilized. Likewise, lighter coveracJe may be obtained by usiny a higher dilution of methanol.
The pigment toning material which is applied as a spray blend to base coated foliage is prepared by utilizing one part oE yellow pigment blend B to four parts of pure methanol. To diminish the intensity of 15 the yellow and to render it more o~ a chartreuse green color, small amounts of the green pigment base A are . subsequently added. ThUs a typical ~ormulation would ; involve one gallon (3.78 liter) o~ pigment B, four gallons (15.14 liters) methanol, and one-half cup (0.12 liter) of pigment blend A.
The actual application of colorant to foliage is a simple direct procsss. The foliage as individual sprigs or as loosely tied bundles is dipped into the base coat blend and swished through this media.
Entrained or adhering air bubbles are so purged from the foliage surPace. Tbe foliage is then shaken to '' ' :

12~5~l~3 drain any excessive film of the colorant base coat blend and immediate:ly hung to dry in an inverted or upriyht configuration which allows good passage oE air provided by natural air movement or enhanced by ~an circulation. At 70F (21~C) and 50~ relative humidity, the base coat dries on most foliages to a state of low-tackiness within five to ten minutes. An addi.tional one-half hour of curing is recommended prior to subsequent toning. Toning, however, may be delayed indefinitely.
In this example, the natural tone blend of yellow is applied by one of two methods utilizing a commercial spray painting meachanism, but may be obtained with any nature of air-assisted, air brush, film application spray gun. Thus, utilizing the blend of toner containing pigment B, methanol, and small amounts of pigment A, a Binks-Vantage~ BB-2 Gun fitted with a nozzle size of 0.015 inch (0.38 mm) i5 fed through a paint pot reservoir of 15 - 35 psig (1.05-2.45 kg/cm2 gauge) within a well ventilated sparkfree paint booth. Individual bunches of foliage are toned to aesthetic standards depending upon individual bunch size and foliage type ov~r two to ten second durations. Individual operators develop varying proficiencies of application of toner. The ~inks series mechanisms involve a fixed paint application , 2~
spray cone and operate at variable air assisted pressure. Alternatively, utilizing the same toner blend, an air-over-fluid standard paint gun with pain-t feed ~rom pressure pot will prove functional. Any S spray gun possessing variabl~e flow and variable pattern parameters, and preferably having an external paint mix mechanism, provides satisfactory results.
Immediately a~ter spraying, the toned ~oliage bundles are laid on ~lat racks, or they can be directly hung. Within seconds a~ter application the toner has dried to insiynificant tackiness so that individual bundles of ~oliage or individual sprigs o~
foliage do not adhere to each other or disrupt the finish by contact. However, at 70 (21C) an additional thirty minutes of drying time on such flat racks is allowed prior to packaging. Alternatively, the toned foliage bundles or individual sprigs may be attached to a mobile conveyor in a heated, 110F
(43C), air drying tunnel and within less than three minutes the material exits the tunnel, ready for packaging. Individual bundles are bagged in polypropylene clear bags according to shipment scale design and twist-tie sealed.
As described in the above example, the coating so applied renders the foliage natural and lifelike in color and inhibits transpiration of entrained ' ' .

~ , humectants. Its shelf life under the conditions of production are significantly improved due to the application of the base coating and its sealant components of adhesive or anki-transpirant such as outlined above. Numerous other possible combinations of antitranspirants or sealing adhesives are feasible for this process.
Foliage which is to be rendered bleached of color due to sun bleaching after preservation in ethylene glycol is likewise dipped with a sealant.
The preferred sealant blend is a combination involving the Fuller Adhesive X-3801 or Agro-K Corporation Envy-Antitranspirant~ blended with twice the volume of Aquo-Mac~ 607 or 609 Acrylic Media and subsequently diluted with an equal volume of water. This in turn i5 then diluted with ten parts by volume of methanol.
The total milky dispersant blend is utilized as a dip on the buckskin line of foliage and allowed to air dry in identical fashion ko the pigment application base coat. No additional colorant need be added. However, if pure white foliage is to be produced, such a transparent base coat is subsequently oversprayed with any variety of Tikanium White-600 tone coatings by spray application. A typical tone coating by spray applications would involve a blend of one cup ~0.24 liter) of Titanium White-600 dispersed in one cup ~.

~28~;3 (0.24 liter) of water which in turn is added to one gallon (3.78 liter) of Aquo-Mac and one-half gallon (1.89 liter) of Antitranspirant or Adhesive 3801 and diluted with ten gallons (37.8 liters) of methanol.
White toning is applied in similar fashion to that described for the application of the natural chartréuse green toning color.
The above are simple examples; numerous other possible color combinations may be applied using various varieties and classes of pigments. Thus, for example, foliage may be produced of a red, pink, yellow, blue, gold, silver, orange, or any other natural or unnatural blend of colors.
Although the two-step process of sealing and tinting described thus far works well with all types of foliage materials, most foliage types may be effectively sealed and tinted in a single step with a hydrophilic blend of polymer and pigment. Other possible components may include extenders, dispersants, thickeners, solvents, antifoam agents and pH control agents. This topical coating is most easily applied as a dip-coat, but it may also be applied by spraying. The hydrophilic nature of the blend is most critical to ensure adhesion to the effectively wet foliage surface having ethylene glycol adhering to it.

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The following exemplary one-step Formulation A
renders preserved foliage natural in color and general appearance, and uses a green pigment latex which provides uniform coverage and a depth of tone which masks all decolorization effects resulting from the preservation process. The polymer latex vehicle is used to disperse and overlay the foliaye in a film.
For this purpose, we have found that vinyl acetate/hydroxyethyl acrylate copolymers having an average range of molecular weights of 30,000 are the preferred filming agents.

Formulation A for Latex Green_~a~e Coat Inqredient Ran e Percent by Weiaht Function Chrome Green (Cr203) 10.0 - 30.0 Pigment Water Cround Mica 1.50 - 5.00 Extender Sodium Polyphosphate 0.50 - 1.00 Dispersant Sodium Carboxymethyl Cellulose 0.30 - 0.70 Thickener Methocel~ Antifoam 0.02 - 0.10 Antifoam Ammonia t0.88 H20 solution) 0.01 - 0.07 Alkalinity control Butylacetate 2 ~ 3 Coalescing solvent Vinylacetate/
Hydroxyethyl ,~, :

35~53 Acrylate/Acrylic Acid 45:45:10 Copolymer (50% solids in H2O
dispersion) 30.0 - 45.0 Film former Water 30.0 - 45 0 100. 00 This formulation effectively masks the unnatural faded greyish-green appearance of the foliage resulting from preservation with humectant ethylene glycol. The chrome green pigment pleasingly matches the natural color of many foliages. Other pigments are used to achieve whatever tint is desired.
Additional artistic effects may be obtained by further steps of spraying or dip-coating.
Another example of an effective hydrophilic one-step blend is shown as Formulation B, which is in the form of a water latex dispersed emulsion. The formulation is colorless without added pigment.
Pigment is added to the formulation to obtain coloration, and is selected to achieve the desired aesthetic effect in the final coated foliage materials.

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Formulation ~ ~or Latex Emulsion Base Coat-Colorle~s for Pigment Blends Inqredient Ranqe Percent by Weiqht Function Pigment - inert and variable in blends (not part of wt%) Talc or Water ground mica 7.0 - 15.0 Extender Tamol~ 731 1.50 - 2.50 Surfactant (Rohm and Hass) Methocel~ Antifoam 0.10 - 0.30 Antifoam Hydroxyethyl Cellulose 0.20 - 0.50 Thickener Butylacetate1.00 - 3.00 Coalescing Solvent Ammonia (0.88 H20 Solution) 0.02 - 0.07 Alkalinity Control Vinylacetate/Vinyl "Versatate"~
55:45 Copolymer (52~ solids in H20 dispersion)40.0 - 60.0 Film Former Water 25.0 - 40.0 100.00 The indicated percentage component ranges are exemplary only, and are not intended to be limiting.
Furthermore, all of the listed components in Formulation A and B need not be used in a particular blend. For example, an alkalinity control agent is not always necessary.

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5~5i3 Following the application oE Formulations A or B
or similar blends, foliage may be enhanced in aesthetic e~fect by further steps of spraying or dip-coating with a wide variety of colored or clear coating materials.
Plant materials treated according to the present invention retain the flexibility of their freshly cut state. The strength is retained or enhanced, resulting in a long shelf life and a long useful life for decorative, scientific or display purposes.
Furthermore, dust and grime adhering to the plant materials as a result of storage or exposition may be easily removed by washing with cool or cold water, optionally containing a weak nonionic detergent or castile soap, to restore the materials to a clean, aesthetically attractive state.

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Claims (35)

1. A method for preserving natural plant materials, including cut foliage, comprising the steps of:
(a) immersing a batch of said plant materials in a starting volume of ethylene glycol having a specific gravity of 1.03 to 1.10 at a pressure of about 3 to about 30 psig (0.21 to 2.1 kg/cm2 gauge) for a period of four hours to five days to effect exchange of plant fluids in said plant materials with said ethylene glycol and produce treated plant materials;
(b) withdrawing said treated plant materials from the pressurized immersion in the spent ethylene glycol;
(c) washing excess ethylene glycol from the surface of said treated plant materials;
(d) drying said treated and washed plant materials;
(e) adding ethylene glycol having specific gravity no lower than 1.03 to said spent ethylene glycol from step (b) to restore the starting volume; and (f) preserving a further batch of said plant materials in said restored starting volume of ethylene glycol in accordance with steps (a) - (e).
2. The method according to claim 1, wherein said immersed bath of plant materials is periodically or continuously agitated to expel gas bubbles therefrom.
3. The method according to claim 1, comprising the further step of immersing said treated plant materials in ethylene glycol having a specific gravity of 1.05 - 1.10, for up to one week at atmospheric pressure, before washing step (e).
4. The method according to claim 1, comprising the further step of exposing said washed and dried plant material to sunlight for 20 to 100 hours to produce material having a pale buckskin tan coloration.
5. The method according to claim 4, comprising the further step of coating said washed and dried plant material with a sealant prior to or following sunlight exposure.
6. The method according to claim 1, comprising the further step of sealing said dried plant materials from step (d) to prevent bleed-out of ethylene glycol and enhance the shelf life and utility of said plant materials.
7. The method according to claim 6, wherein said sealing comprises dipping said dried plant materials into a blend of an acrylic baser water and a water dispersible adhesive or polymeric antitranspirant.
8. The method according to claim 1, comprising the further steps of dipping said dried plant materials from step (d) into an acrylic base and glue subcoating to seal and to mask the color of said materials, removing and drying said subcoated materials, and spray painting with one or more color pigments blended with a water dispersible adhesive or polymeric medium to tint said materials.
9. Natural plant materials treated according to the process of claim 8, wherein said materials contain ethylene glycol of specific gravity 1.025 to 1.10, sealed within said materials by an acrylic base and glue subcoating, and are spray painted with one or more pigments blended with a water dispersible adhesive or polymeric medium.
10. The method according to claim 1, comprising the further step of topically coating said dried plant materials from step (d) with a tinting sealer comprising a hydrophilic blend of polymer and pigment.
11. The method according to claim 10, wherein said polymer comprises a vinyl acetate/hydroxyethyl acrylate copolymer.
12. Natural plant materials treated according to the process of claim 10, wherein said materials contain ethylene glycol of specific gravity 1.025 to 1.10 sealed within said materials by a tinting sealer comprising an hydrophilic blend of polymer and pigment.
13. A method for preserving natural plant materials, including cut foliage, comprising the steps of:
(a) immersing a batch of said plant materials in a starting volume of ethylene glycol having a specific gravity of 1.05 to 1.10 at a pressure of about 3 to about 30 psig (0.21 to 2.1 kg/cm2 gauge) for a period of one to five days to effect exchange of plant fluids in said plant materials with said ethylene glycol and produce treated plant materials;
(b) withdrawing said treated plant materials from the pressurized immersion in the spent ethylene glycol:
(c) washing excess ethylene glycol from the surface of said treated plant materials;
(d) drying said treated and washed plant materials;
(e) adding virgin ethylene glycol to said spent ethylene glycol from step (b) to restore the starting volume, and (f) preserving a further batch of said plant materials in said restored starting volume of ethylene glycol in accordance with steps (a) - (e).
14. The method according to claim 13, comprising the further step of immersing said treated plant materials in ethylene glycol having a specific gravity of 1.05 - 1.10. for up to one week at atmospheric pressure, before washing step (c).
15. The method according to claim 13, comprising the further step of exposing said washed and dried plant material to sunlight for 20 to 100 hours to produce material having a pale buckskin tan coloration.
16. The method according to claim 15, comprising the further step of coating said washed and dried plant material with a sealant prior to or following sunlight exposure. ]
17. The method according to claim 13, comprising the further step of sealing said dried plant materials from step (d) to prevent bleed-out of ethylene glycol and enhance the shelf life and utility of said plant materials.
18. The method according to claim 17, wherein said sealing comprises dipping said dried plant materials into a blend of an acrylic base, water and a water dispersible adhesive or polymeric antitranspirant.
19. The method according to claim 13, comprising the further steps of dipping said dried plant materials from step (d) into an acrylic base and blue subcoating to seal and to mask the color of said materials, removing and drying said subcoated materials, and spray painting with one or more color pigments blended with a water dispersible adhesive or polymeric medium to tint said materials.
20. Natural plant materials treated according to the process of claim 19, wherein said materials contain ethylene glycol of specific gravity 1.05 to 1.10, sealed within said materials by an acrylic base and glue subcoating, and are spray painted with one or more pigments blended with a water dispersible adhesive or polymeric medium.
21. The method according to claim 13, comprising the further step of topically coating said dried plant materials from step (d) with a tinting sealer comprising an hydrophilic blend of polymer and pigment, to seal and color said plant materials in a single topical application.
22. A method for preserving natural plant materials, including cut foliage, comprising the steps of:
(a) placing a batch of said plant materials in a pressure vessel;
(b) introducing ethylene glycol having a specific gravity of 1.03 to 1.10 from the bottom of said pressure vessel with a strong flow to remove gases clinging to said plant materials and gases entrained in said ethylene glycol, until said pressure vessel is filled with said plant materials immersed in ethylene glycol essentially free of gases;
(c) sealing said pressure vessel and pressurizing to an internal pressure of about 3 to about 30 psig (0.21 to 2.1 kg/cm2 gauge) without introducing gases into said vessel;
(d) maintaining said plant materials at said pressure for four hours to five days to effect exchange of plant fluids in said plant materials with said ethylene glycol and produce treated plant materials;
(e) withdrawing said treated plant materials from the pressurized immersion in the spent ethylene glycol;
(f) washing excess ethylene glycol from the surface of said treated plant materials;
(g) drying said treated and washed plant materials;
(h) adding ethylene glycol having a specific gravity no lower than 1.03 to said spent ethylene glycol from step (e) to restore the starting volume; and (i) preserving a further batch of said plant materials in said restored starting volume of ethylene glycol in accordance with steps (a) - (h).
23. The method according to claim 22, comprising the further step of adding an antifoaming agent to said starting volume of ethylene glycol.
24. The method according to claim 23, wherein said antifoaming agent has a silicone base.
25. The method according to claim 22, wherein said immersed batch of plant materials is periodically or continuously agitated to expel gas bubbles therefrom.
26. The method according to claim 22, comprising the further step of immersing said treated plant materials in ethylene glycol having a specific gravity of 1.05 - 1.10, for up to one week at atmospheric pressure, before washing step (f).
27. The method according to claim 22 comprising the further step of exposing said washed and dried plant material to sunlight for 20 to 100 hours to produce material having a pale buckskin tan coloration.
28. The method according to claim 27, comprising the further step of coating said washed and dried plant material with a sealant prior to or following sunlight exposure.
29. The method according to claim 22, comprising the further step of sealing said dried plant materials from step (g) to prevent bleed-out of ethylene glycol and enhance the shelf life and utility of said plant materials.
30. The method accoring to claim 29, wherein said sealing comprises dipping said dried plant materials into an hydrophilic blend of an acrylic base, water and a water dispersible adhesive or polymeric antitranspirant.
31. The method according to claim 30, wherein said sealing comprises topically coating said plant materials with an hydrophilic blend of polymer and pigment to seal and color said plant materials.
32. The method according to claim 31, wherein said polymer comprises a vinyl acetate/hydroxyethyl acrylate copolymer.
33. Natural plant materials treated according to the process of claim 31, wherein said materials contain ethylene glycol of specific gravity 1.025 to 1.10, sealed within said materials by an hydrophilic blend of polymer and pigment, said pigment coloring said plant materials.
34. The method according to claim 22 comprising the further steps of dipping said dried plant materials from step (d) into an hydrophilic polymer base and glue subcoating to seal and to mask the color of said materials, removing and drying said subcoated materials, and spray painting or dip-coating with one or more color pigments blended with a water dispersible adhesive or polymeric medium to tint said materials.
35. Natural plant materials treated according to the process of claim 34, wherein said materials contain ethylene glycol of specific gravity 1.025 to 1.10, sealed within said materials by an hydrophilic polymer base and glue subcoating, and are spray painted with one or more pigments blended with a water dispersible adhesive or polymeric medium.
CA 533063 1986-07-25 1987-03-26 Method for foliage and other plant material preservation and topical color application to same Expired CA1285153C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US889,253 1986-07-25
US06/889,253 US4664956A (en) 1985-09-18 1986-07-25 Method for foliage and other plant material preservation and topical color application to same

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CA1285153C true CA1285153C (en) 1991-06-25

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