GUM FOR CIGARETTE PAPER, CIGARETTE PAPER AND METHOD FOR THE PRODUCTION THEREOF
Patent Information
- Application Number
- DE602021032967
- Authority / Receiving Office
- DE · DE
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2020-10-29
- Filing Date
- 2021-10-21
- Publication Date
- 2025-06-25
- Estimated Expiration
- 2041-10-21
AI Technical Summary
Existing methods for incorporating cannabinoids into rolling papers and gum face challenges such as miscibility issues between water and oil, limited cannabinoid quantity, degradation of adhesive properties, and instability of physicochemical properties, leading to staining and compromised manufacturing.
A gum solution for rolling cigarette paper is developed, comprising a mixture of cannabinoids and edible oil, with a controlled proportion of edible oil (0-80% by mass) and plant exudates like gum arabic, allowing for the incorporation of cannabinoids like CBD, CBG, CBC, CBE, and cannabinol, which are soluble in oil, ensuring adhesive properties and stability.
The solution enables controlled and efficient introduction of cannabinoids into cigarette paper, maintaining adhesive properties and stability over time, while adhering to national regulatory limits, enhancing the smoking experience with both flavor and aroma.
Description
DOMAINE TECHNIQUE DE L'INVENTION
[0001] The technical field of the invention is that of rolling cigarette papers and more particularly the adhesive thread used to stick the cigarette paper by reactivation by licking, also called gum used to stick the cigarette paper, its manufacturing process and the cigarette paper obtained. ARRIERE-PLAN TECHNOLOGIQUE DE L'INVENTION
[0002] To improve the smoking experience, the introduction of recreational products into cigarettes has been developed. These recreational products are introduced into the paper itself. There have also been plans to introduce them into the gum core of rolling papers.
[0003] However, recreational products such as cannabinoids, particularly cannabidiol or CBD, are only soluble or miscible in oil, and rolling papers and gum are made from aqueous solutions. Water and oil are not miscible, making it difficult to produce these cannabinoid-enriched rolling papers.
[0004] On the other hand, the authorized rate of cannabinoids is limited depending on the country for non-pharmaceutical uses, it is important to be able to regulate in a controlled and easy way the CBD intake for a rolling paper.
[0005] To address these difficulties it has been proposed to deposit the recreational product on the paper with a fixing agent, however the quantity of product deposited is limited.
[0006] Paper has also been infused with cannabinoids obtained from an oil extract of the cannabis plant, as in US2018 / 360103, US2019 / 390408, and WO2017 / 196840. Because the cannabis extract containing cannabinoids is an oil that is not miscible in water, an emulsifier must be used to allow the cannabinoids to disperse evenly in the papermaking process. These emulsions are additives that complicate the formulation of the paper and make it less natural.
[0007] The introduction of cannabinoids into gum, although envisaged, has never been technically described, notably in document US2020 / 128872.
[0008] All these solutions have the following disadvantages: cannabinoids or oil can cause stains to appear on the sheet of paper if its proportion is too high in the gum, cannabinoids or oil can degrade the adhesive properties of the gum, cannabinoids or oil modify the physicochemical properties such as the rheological properties of the gum, which can impact its manufacture and implementation, the stability over time of the properties of the gum can vary depending on the quantity of cannabinoids or oil introduced, the quantity of recreational product introduced is limited. RESUME DE L'INVENTION
[0009] The invention provides a solution to the problems mentioned above by allowing the introduction of cannabinoids into an adhesive solution. The cannabinoids used can, for example, be chosen pure or mixed from the following cannabinoids: cannabidiol (CBD, 2-[(1R,6R)-6-Isopropenyl-3-methyl-3-cyclohexen-1-yl]-5-pentyl-1,3-benzenediol, C 21 H 30 O 2 , CAS number 13956-29-1), Cannabigerol (CBG, 2-[(2E)-3,7-Dimethyl-2,6-octadien-1-yl]-5-pentyl-1,3-benzenediol, C21H32O2, CAS number 25654-31-3), Cannabichromene (CBC, C21H30O2, 2-Methyl-2-(4-methyl-3-penten-1-yl)-7-pentyl-2H-chromen-5-ol, CAS number 20675-51-8), cannabielsoin (CBE, C21H30O3, 6-Methyl-3-pentyl-9-(prop-1-en-2-yl)-5a,6,7,8,9,9a-hexahydrodibenzo[b,d]furan-1,6-diol, CAS number 52025-76-0) cannabinol (CBN, 6,6,9-trimethyl-3-pentyl-6H-benzo[c]chromen-1-ol, CAS number 521-35-7).
[0010] The adhesive solution can be made from natural plant compounds, more or less branched polyoses, plant exudates, extracts of seeds, fruits, cereals, possibly mixed together at measurable rates. They can be chosen from the following plant exudates: gum arabic constituent monomers Galactose-Arabinose-Rhamnose-Glucuronic acid, gum ghatti Arabinose-galactose-mannose-xylose-glucuronic acid, gum karaya constituent monomers rhamnose-galactose-galacturonic acid, fruit extracts, gum pectins constituent monomers galacturonic acid-rhamnose-galactose-arabinose-xylose, seed extracts; guar gum based on galactose and mannose, blackberry gum consisting of galactose-mannose, seaweed extracts Agar, alginates and carrageenans; cereals and tubers, starches of wheat, corn, sorghum, potato, constituent monomer glucose.
[0011] A first aspect of the invention relates to a gum of plant origin, for rolling cigarette paper comprising a defined percentage of dry extract, said gum is characterized in that it comprises a mixture of cannabinoids and edible oil, the edible oil being present in the mixture in a proportion p such that 0% ≤ p ≤ 80% by mass of the mixture. The cannabinoids being soluble only in the oil and the gum being intended to be brought to the mouth since it must be re-activated by licking once coated, smoked and swallowed, it is necessary to use a minimum of the oil and for it to be edible. The gum may, for example, be gum arabic initially in solid form, dissolved essentially in water with incorporation of various possible additives.This highly branched polysaccharide is edible and the resulting mucilaginous solution with high dry extract is used here for its adhesive properties, it is intended for the area coating of rolling cigarette paper, the mucilaginous solution is ready to use.
[0012] Throughout the rest of the description, the percentages indicated are percentages by mass of the compounds concerned in the ready-to-use formulation. The dry extract (SE) corresponds to the material remaining when all the water has been removed from the preparation.
[0013] Advantageously, the maximum quantity of edible oil in the gum is limited to 20% by mass of the dry extract of the gum, preferably less than 16% by mass of the dry extract of the gum. With this proportion, the risks of the oil in the gum separating over time are controlled.
[0014] According to a first embodiment, the cannabinoid is crystallized CBD and the edible oil is present in the mixture with a proportion p such that 20 ≤ p ≤80% by mass of the mixture. This crystallized CBD is 99% pure, which makes it possible to optimize the quantity of CBD introduced into the gum.
[0015] In a second embodiment, a crude apolar cannabis extract - herein referred to as broad spectrum CBD - was used with or without oil and the edible oil is present in the mixture with a proportion p such that 0% ≤ p ≤ 20% by mass of the mixture. The broad spectrum CBD may be derived from a crude cannabis extract with supercritical CO2 and then partially refined according to national legislation. Broad spectrum CBD requires less oil, or even almost no oil, and is therefore easier to incorporate into the gum. Broad spectrum CBD is free of THC (Tetrahydrocannabinol).
[0016] Advantageously, the edible oil is hemp oil. Hemp oil has the advantage of containing few saturated fatty acids, which are not very fluid, and many polyunsaturated fatty acids, which are very fluid. It is therefore naturally very fluid at 20°C, which is a definite advantage for dispersing the oil containing the cannabinoids in the gum juice. It is indeed important that the oil is not solid at room temperature.
[0017] Other oils can be selected from the following: all vegetable oils for food use, such as olive, rapeseed, grape seed, sunflower oil, which are relatively fluid or possibly palm, coconut which are more viscous depending on production needs and / or market availability.
[0018] Advantageously, the dry extract comprises a plant exudate, preferably an acacia or gum arabic exudate.
[0019] According to a first option, this acacia exudate is preferably composed of 70% to 30% of Senegal variety and 30% to 70% of Seyal variety. The composition of 70% Senegal variety and 30% Seyal variety allows to obtain the best results in its suitability for machine passage and adhesiveness at a controlled cost. It is possible to limit costs by going up to 70% of Seyal variety in gum arabic by depositing more gum on the paper, because Senegal acacia, of better quality, is more expensive than Seyal acacia.
[0020] A second option is to use gum arabic made from 100% Seyal, reducing the cost.
[0021] A third option is to use 100% Senegal gum arabic, which gives the best results.
[0022] A second aspect of the invention relates to a rolling cigarette paper comprising gum with at least one of the preceding characteristics. The cigarette obtained by rolling the gummed cigarette paper allows the smoker to enjoy the aroma of cannabis both when licking the paper to activate the stickiness and while smoking.
[0023] According to a first variant, the gum is in the form of a net. The width of the gum net can be between 3mm and 15mm, preferably between 5mm and 10mm. The quantity of adhesive gum deposited by reactivation can vary between 30 and 60 mg / m over 5mm width. It is thus possible to vary the quantity of cannabinoid in the gummed paper.
[0024] In a second variant, the gum is in the form of a print. The gum is deposited using a printing process, which allows it to be given any desired shape. The coating area can be made by longitudinal or transverse thread, continuous or discontinuous, or in the form of patterns distributed over more than 30% of the surface of the cigarette paper sheet, which further increases the quantity of cannabinoids on the same gummed paper.
[0025] A third aspect of the invention relates to a method for producing a gum with at least one of the preceding characteristics, obtained from a gum juice and comprising the following steps: introduction of a mixture of cannabinoids and edible oil, the edible oil being present in the mixture with a proportion p such that 0% ≤ p ≤ 80% by mass, incorporation into the water of additives dissolution and dissolving in the water of a dry extract composed of all the solid matter contained in the gum juice drying of the gum juice.
[0026] Incorporating the oil before or after the gum arabic powder into the water has little impact on the stability of the gum. However, stability appears to be slightly better when the cannabinoids are incorporated before the gum powder. The dissolution of the dry extracts and the introduction of the oil is done by stirring the mixture for approximately 30 minutes under vacuum in a reactor.
[0027] Advantageously, broad-spectrum CBD with or without oil is heated to 70°C before being introduced into the gum juice. Broad-spectrum CBD is heated to 70°C in the presence or absence of oil before being introduced into the reactor. This makes broad-spectrum CBD more fluid and easier to incorporate into the gum juice.
[0028] Advantageously, the gum is stirred and heated to 70°C until the cannabinoid is completely diluted for homogeneous incorporation. Heating the gum juice facilitates the incorporation of the cannabinoid-enriched mixture into the gum juice.
[0029] Advantageously, the gum juice has a dynamic viscosity at 22°C of between 65 seconds and 115 seconds, preferably between 85 and 92 seconds. This dynamic viscosity is measured with an Afnor T30.014 viscosity cup; this cup is a flow cup used to determine the flow time of a volume of liquid through a calibrated orifice and is measured in seconds of flow. In the present invention, the cup has a diameter of 50mm and a height of 44mm with an orifice of diameter 5.8mm. Increasing the oil content decreases the viscosity while increasing the dry extract content increases it; the balance between these two components makes it possible to obtain the desired viscosity for the given process.
[0030] Advantageously, the gum juice contains between 37% and 45% dry extract. This percentage allows the desired viscosity to be obtained. For crystallized CBD, the SE of the gum juice will preferably be 41.0% and for broad-spectrum CBD, the SE of the gum juice will preferably be 40.7%.
[0031] Advantageously, the amount of exudate is greater than 75% by mass in the ES. This amount is necessary to ensure good paper bonding.
[0032] The various aspects of the invention will be better understood by reading the following description and examining the accompanying figures. BREVE DESCRIPTION DES FIGURES
[0033] The figures are presented for information purposes only and in no way limit the invention. [ Fig. 1 ] is a view of a rolling cigarette paper, [ Fig. 2 ] is a chart of the flow time of a liquid for a given volume under specific temperature and pressure conditions called the dynamic viscosity of a gum juice as a function of the quantity of dry extract (SE), [ Fig. 3 ] shows the evolution of the dynamic viscosity of the gum juice over time as a function of the percentage of dry extract in the presence of 9.11% oil, [ Fig. 4 ] shows the evolution of the dynamic viscosity of the gum juice over time as a function of temperature with a dry extract with a constant oil portion at 9.11% in the dry extract, [ Fig. 5 ] illustrates the variation of the dynamic viscosity of the gum juice as a function of the quantity of dry extract and its evolution over time, [ Fig. 6 ] shows the evolution of the dynamic viscosity of the gum juice over time as a function of the percentage of dry extract at constant oil proportion in the ES, [ Fig. 7 ] illustrates the variation of dynamic viscosity of gum juice over time depending on different types of compounds dissolved in the oil at 41% ES and 9.11% oil in the ES, [ Fig. 8 ] illustrates the variation of the dynamic viscosity of the gum juice as a function of the quantity of oil at a constant dry extract percentage of 43%, [ Fig. 9 ] shows the stability of gum juice at fixed ES and increasing oil content, [ Fig. 10 ] is a table showing the different modes of introduction of broad spectrum CBD, [ Fig. 11 ] shows the evolution of the dynamic viscosity of the gum juice over time as a function of the temperature of introduction of the broad-spectrum CBD into the gum juice and the mixing temperature, [ Fig. 12 ] represents the dynamic viscosity of the oil as a function of the temperature of introduction of the broad spectrum CBD into the gum juice and the mixing temperature of the robot, [ Fig. 13 ] shows the application of the gum to the paper and its drying in the oven, [ Fig. 14 ] is a top view of the oven and paper rolls, [ Fig. 15 ] is a table showing the results of paper gumming according to different modes of introduction of CBD crystals and broad-spectrum CBD into the adhesive preparation, [ Fig. 16 ] is a graph illustrating the evolution of the viscosity of different rubber mixtures. DESCRIPTION DETAILLEE
[0034] The various tests were conducted with CBD, but the chemical structures of the different cannabinoids are relatively close to each other, meaning that their physicochemical properties are also similar. All cannabinoids are very non-polar and therefore very poorly soluble in water. The behaviors of these cannabinoids are very similar to those observed and measured for CBD.
[0035] The gum is first made in the form of a mucilaginous solution, here called gum juice, which is placed on the cigarette rolling paper, then dried. The dried gum must be soft enough not to crack and become sticky by wet reactivation of saliva to make the cigarette. Rolling paper 1, illustrated figure 1 , shows a line of gum 2 placed along the entire length of one of the edges of the rolling paper 1.
[0036] The gum juice according to the invention is composed of water, a humectant such as sorbitol, optionally caramel quality E150 (a), a branched polysaccharide such as gum arabic alone or in a mixture with other natural vegetable gums, plant exudates, extracts of fruits, seeds or algae, cereals or tubers, a cannabinoid. and optionally vegetable oil. The various components are solubilized in water or suspended in water. Sorbitol allows the gum to maintain a certain elasticity to prevent it from cracking after drying the gum juice, and it improves adhesion. Caramel or E150 is a coloring agent, used here to give contrast to the gum line compared to the sheet and distinguish the location of the adhesive line. Gum arabic is, for proportions ≥ 30% Senegal, a very powerful natural adhesive.The oil helps facilitate the dispersion or incorporation of the cannabinoid into the gum juice.
[0037] The dry extract is therefore composed of all the solid matter contained in the gum juice.
[0038] The gum juice is deposited onto the paper through the nozzle of a gumball machine to deposit a stream of gum of a consistent width onto the rolling paper. This width can be chosen between 5 and 15mm, and it is also possible to deposit several streams of gum. The stream is relatively narrow. ilIt is necessary that the gum juice has a certain viscosity to pass through the nozzle with a flow rate suitable for industrial production. It is also important that the gum juice becomes stable, so storage of at least 24 hours is necessary and that it remains stable over time so that it can be stored for at least 72 hours before use. It is known that these preparations, made with more or less branched and networked long-chain polymers, are bulky and very polydisperse, and they require 24 hours of reorganization before being put into production and having stable rheological behavior on the machine. This phenomenon is potentially accentuated by the addition of CBD and oil.
[0039] Dynamic viscosity measurements of the gum juice were carried out as a function of the percentage of dry extract, the quantity of oil and the evolution over time, with the objective of a dynamic viscosity between 80s and 95s at 22°C.
[0040] The abacus of the figure 2 was made with a standard gum juice composed of water, acacia powder made up of 70% Senegal variety and 30% Seyal variety, sorbitol and caramel.
[0041] We can see on this chart that at time t 0 when the gum juice is made, the curve t 0 representing the dynamic viscosity increases with the percentage of dry extract (SE). The variation of the viscosity was measured over time at 24h (t 24 ), 48h (t 48 ), 72h (t 72 ) and at 86h (t 86 ). We note a strong change in viscosity over time between t 0 and t 24 . Thus from 24h after the gum is made the measurements fluctuate slightly. The viscosity has decreased (curve t 24 ) and continues to decrease at 48h (curve t 48 ) to increase again at 72h (curve t 72 ) and finally decrease after 86h (curve t 86 ). This chart shows that increasing the dry matter content by 1% results in an increase in dynamic viscosity of 15s. The dynamic viscosity target is set between 80s and 95s.The dynamic viscosity target is set so that the gum juice can be passed through a gum press and have a stable / defined amount of gum solids on the finished product (rolling paper sheet).
[0042] The flow of juice delivered by the gum machine is indexed to the paper running speed. The gum juice must be fluid enough to pass through the gum machine's supply pipes but not too fluid so as not to wet the paper too much, because humidity weakens the paper which can cause potential breakages during erasing (placing the gum on the paper) and so that the gum is dry when it leaves the drying oven. Indeed, as the paper is rewound when it leaves the drying oven, if the gum is still wet when it leaves the gum machine, the reel produced will be stuck and cannot be unwound for the following stages of notebook manufacturing.
[0043] There figure 3 shows the evolution over time of the viscosity as a function of the ES rate with a stable oil percentage at 9.11%. The evolution over time of the viscosity as a function of the dry extract percentage between 39% and 43% was measured, with a fixed oil quantity at 9.11% in order to establish a rule to be applied when increasing the dry extract percentage by 1%. The measurement was made at 0, 3 and 9 days. The results at 0 days (curve T 0 ) are not homogeneous, on the other hand at 3 days (curve T 3 ) and at 9 days (curve T 9 ), the curve is practically straight and allows us to deduce that, here too, a variation of 1% of dry extract increases the viscosity by approximately 15s between 39% and 43% ES.
[0044] There figure 4 shows the variation of viscosity as a function of temperature from the measurement of two identical juices but made by incorporating the oil before the acacia powder A1 or after the powder A2. We can see that there is no significant difference, the decrease in viscosity has a constant slope almost identical with an average A3. We can deduce that a variation of +1°C in temperature leads to a variation of -2.5s in dynamic viscosity and conversely a variation of -1°C in temperature leads to a variation of +2.5s in dynamic viscosity.
[0045] There figure 8 shows the variation over time of the viscosity of the gum juice as a function of the quantity of oil with a constant percentage of dry extract of 43% in order to evaluate its stability. These measurements were made in order to verify whether it was possible to significantly increase the oil content in the gum juice and therefore the quantity of solubilized CBD powder over 8 days. The proportion of oil in the gum varied between 9.11% and 44.44%: Curve H1 corresponds to an oil proportion of 9.11%, Curve H2 corresponds to an oil proportion of 16.7%, Curve H3 corresponds to an oil proportion of 28.62%, Curve H4 corresponds to an oil proportion of 44.5%,
[0046] We can thus see that the juices are stable for 8 days after at least 24 hours. However, a phase shift was observed on the 28% gum juices (H3) from +24 hours, so it was rehomogenized. The 44% juice (H4) has completely phase shifted and is very slightly adhesive. Here, the limiting oil percentage is therefore less than 28% of the dry extract.
[0047] There figure 9 illustrates the variation of viscosity as a function of the percentage of oil in the juice and its evolution over time at 0 (d0), 3 (d3) and 8 days (d8). It can be seen that the viscosity decreases when the quantity of oil increases, but that from 25% oil (reference L3) the viscosity of the oil is no longer linear and that from 28% oil (reference L4), the juice begins to separate. The limit of the proportion of oil in the preparation is therefore 25%, preferably less than 20% of the ES.
[0048] We can see figure 6 the evolution over time of dynamic viscosity measurements of juice with a constant oil percentage of 9.11% with a variable ES rate of 39 to 43%. By varying the percentage of dry extract for a given quantity of oil of 9.11% and we measure the evolution of the kinetic viscosity over time. The measurements were carried out with the products ES1, ES2, ES3, ES4 and ES5 below. We note that the gum juice of all of these products is quite stable over time after 24 hours and predictably, the dynamic viscosity increases with the percentage of dry extract. The percentage of ES at 41% was chosen because it has the desired viscosity.
[0049] Measurements with 40% to 43% dry extract and 9.11% to 28.62% oil were carried out, corrected and are visible on the figure 5 . The measurements were made with the following compositions: ES1: 43% dry extract and 9.11% oil, ES2: 42% dry extract and 9.11% oil, ES3: 41% dry extract and 9.11% oil, ES4: 40% dry extract and 9.11% oil, ES5: 39% dry extract and 9.11% oil, ES6: 43% dry extract and 16.69% oil, ES7: 43% dry extract and 28.62% oil, ES8: 41% dry extract and 9.11% oil.
[0050] The ES1, ES2, ES4, ES5 and ES8 measurements were then corrected for a simulation at 41% dry extract. Thus the ES1 measurement was corrected by removing 30s, the ES2 measurement by removing 15s, the ES4 measurement by adding 15s, the ES5 measurement by adding 30s. The ES8 measurement was calculated from viscosity measurements of two juices: one at 42% ES and the other at 39% ES, each corrected to be reported at 41% ES; each measurement point of these juices allows the production of a curve at 41% ES, therefore with a loss of viscosity of 15 seconds compared to the results measured for the juice whose ES was 42% and a gain of 30 seconds for the juice whose ES was 39%. Finally, the ES7 measurement was corrected by adding 30 seconds to the values to target an ES of 45%. This allows us to compare the evolution over time of the kinetic viscosity of the different concentrations of dry extract.We note that there is little dispersion, the dynamic kinetic viscosity remains between 80s and 95s.
[0051] Composition ES1, which has too high a viscosity, is not retained.
[0052] When the amount of oil is increased from 9.11% to 16.69%, the amount of dry extract must be increased to maintain the same viscosity; its percentage therefore increases to 43%. The measurement results correspond to curve ES6. We see that the viscosity remains within the target range.
[0053] However, when the oil quantity is at 28.62% with a dry extract percentage of 43%, the ES7 curve drops too much, the viscosity is too low, since after 7 days it goes beyond the minimum target and the gum juice gradually separates, that is to say that the water and the oil separate into two phases. The oil quantity is therefore too high.
[0054] There figure 7 illustrates the evolution over time of six gum juices with extrapolated values of 41% ES and 9.11% oil, the results of these curves were recalculated for a target ES of 41% ES and 9.11% oil, then averaged. Three types of gum juice were used for the tests: D0: two with oil alone (one with ES = 39% and one with ES = 42%), D1: two with oil and CBD powder (one with ES = 39% and one with ES = 42%) and, D2: two with oil and menthol (one with ES = 39% and one with ES = 42%).
[0055] This figure shows the influence of CBD on the dynamic viscosity of the gum juice. Curve J0 corresponds to a gum juice with oil without CBD, curve J1 to a gum juice with oil with crystallized CBD and J2 to a gum juice with oil with menthol. Menthol was chosen for its similarity to CBD in terms of hydroxy and methyl groups, terpenes and the same ratio of carbon and oxygen numbers in the crude formula. It can be seen that there is a similarity between curves J0 and J1 from the 1st day. The introduction of crystallized CBD into the oil has little influence on the dynamic viscosity of the gum. CBD is dissolved in the oil by heating it and mixing the mixture under agitation until the crystals disappear.
[0056] Further testing has been conducted with oil-free broad-spectrum CBD made from hemp extract containing approximately 85% CBD and other terpenes capable of providing a particular odor and flavor. Oil-free broad-spectrum CBD can, for example, be obtained from hemp extraction using super-critical CO2 and then semi-purified. This oil-free broad-spectrum CBD is in solid form at room temperature, so it needs to be heated to be introduced into the gum. It is at 60°C that this broad-spectrum CBD becomes liquid. The objective is to find the best compromises to develop a formulation that achieves a satisfactory viscosity over 10 days.
[0057] The table of the figure 10 shows the different broad spectrum CBD introduction processes used: S1 blend without CBD broad spectrum without oil, with a blend made at 30°C and the ES measurement was 41%, S2 blend without CBD broad spectrum without oil, with a blend made at 60°C and the ES measurement was 43%, S3 blend with CBD broad spectrum without oil, heated to 60°C and introduced with a blend made at 30°C and the ES measurement was 40%, S4 blend with CBD broad spectrum without oil, heated to 60°C and introduced with a blend made at 60°C and the ES measurement was 41%, S5 blend with CBD broad spectrum without oil, heated to 60°C and introduced with a blend made at 60°C and the ES measurement was 43%, S6 blend with CBD broad spectrum without oil, not heated at 20°C and introduced with a blend not heated at 20°C and the ES measurement was 43%, S7 blend with broad spectrum CBD without oil, heated to 60°C and introduced with a blend made at 30°C and the ES measurement was 42%, S8 blend with broad spectrum CBD without oil,heated to 70°C and introduced with a mixture made at 70°C and the ES measurement was 41.5%, S9 mixture with broad spectrum CBD without oil, heated to 40°C and introduced with a mixture made at 60°C and the ES measurement was 41%, S10 mixture with broad spectrum CBD without oil, heated to 40°C and introduced with a mixture made at 40°C and the ES measurement was 41%.
[0058] These processes gave the following results: S1 nothing special, S2: the juice foamed enormously. S3: the juice foamed enormously and a surface deposit appeared on the 5th day. S4: The juice foamed enormously and a pedicle appeared on the surface. S5: The juice foamed enormously and a pedicle appeared on the surface at 5 days. S6: The oil-free broad spectrum CBD is very solid so chips were incorporated. After 30 minutes of mixing, the oil-free broad spectrum CBD is still not incorporated. It was stirred again while heating to 60°C, but after returning to room temperature, the presence of oil on the surface and oily points in the mucilaginous preparation was observed. S7: The oil-free broad spectrum CBD cooled quickly and pellets were observed in the gum juice. S8: The juice foamed enormously and the mixture is homogeneous. S9: The juice foamed enormously and the broad spectrum CBD without oil at 40°C, does not liquefy in the mixture at 60°C.S10: The juice has foamed enormously and the broad spectrum CBD without oil at 40°C remains on the blender blade and there are lumps present.
[0059] The viscosity results are visible in graphs 11 and 12. We can see that the viscosities are quite stable over 9 days, that they are between 66 and 105 s with an average of 88 seconds and that there is a slight increase in viscosity over time.
[0060] It is found that the best results are achieved by preheating the oil-free broad spectrum CBD to 60°C before incorporating it into the gum juice to introduce it at this temperature and making the mixture at 60°C.
[0061] We will now describe the application of gum juice to paper using a continuous stream process. However, other processes are possible, such as the flexographic process, where pre-dosing is carried out using an anilox with very specific engraving characteristics that are adapted to the wet quantity to be conveyed onto the paper. The anilox is used to supply a measured quantity of ink or product to the flexographic plate. This preparation can thus be applied to a maximum of 30% of the sheet, plates, discrete patterns, drawings, continuous lines or not.
[0062] As visible figure 13 , the paper 1 is arranged in a roll 10, it is unrolled then nozzles 30 of a gum dispenser 3 deposit the gum juice in a net 2 on the paper which is then passed into an oven 4 where the gum juice is dried. Afterwards, the paper 1 is cut, by knives 5, into strips 12 in the center of the gum net 2 then wound on reels 11. The paper 1 will then be cut into rectangles to make sheets of rolling paper.
[0063] The gumming is carried out with the gummer 3 at a constant speed and at a constant oven temperature 4. The quantity conventionally expressed in dry gum equivalent deposited ranges from 36mg per linear meter for 5mm width to 50mg per linear meter for 5mm width. To increase the quantity of gum deposited from 36mg / m to 50mg / m, the flow rate of the nozzles 30 is increased and / or the gumming speed is reduced by a certain percentage compared to the speed at lower deposit.
[0064] Gum deposition tests on paper were carried out with a mixture of crystallized CBD and with a broad-spectrum CBD.
[0065] The amount of CBD incorporated into the formulation and then deposited on the paper remains less than or equal to 4.62% by mass of the ES in these tests. But if we incorporate 9% of oil comprising 20% of CBD, in the ES, we will obtain 1.8% by mass of CBD in the ES, with 16% of oil comprising 20% of CBD, in the ES, we arrive at 3.2% by mass of CBD in the ES, and with 25% of oil comprising 20% of CBD, in the ES, the CBD rate is 5% by mass in ES. According to national legislation the cannabinoid will not contain THC.
[0066] A summary table showing the manufacturing conditions of the erasers and the results of the erasing tests is presented in figure 15 . Nothing particular was observed for the mixture with crystallized CBD solubilized in the oil. On the other hand, for the broad spectrum CBD, candles or hard filaments formed between the paper at the coating member, this material then accumulated in stalagmites at the nozzle outlet when the dry extract of the adhesive preparation was too high or when the temperature of the broad spectrum CBD was lower than 60°C in the gum juice manufacturing process. Thus, the dry extract of the gum juices is preferably 40.8% but must not exceed 41.7% if hemp oil is not used as an additive. Tests were carried out in the presence and absence of hemp oil in the gum juice. Indeed, the presence of oil made it possible to reduce the phenomenon of candle formation.
[0067] The measurement of S15 juice which is a classic juice does not contain CBD and we can see that its heating during its manufacture does not modify the qualities of the latter.
[0068] In fact, we can see on the table of the figure 15 showing the results of tests on twelve juices P1, P2 and S11 to S20, that juice S11 made at less than 60°C creates candles and that juices S12 and S20 also create some in part and their percentage of dry extract measured is greater than 41.7%. It should be noted that the addition of 5% of oil is not sufficient to completely make the candles disappear (S12) and crystals also appeared.
[0069] Juices P1 and P2 were both made with CBD-enriched oil in a proportion of 22% CBD and 78% oil. For P1, there is 11.6% of the previous enriched oil with a measured ES of 41.20%, or 2.5% CBD in the ES. For P2, there is 21.3% enriched oil with a measured ES of 41.20%, or 4.6% CBD in the ES.
[0070] It can be seen that juices S16 and S17 with a dry extract percentage greater than 41.7% contain 10% oil, which allows scrubbing without the appearance of candles. Although juice S17 was homogenized before scrubbing and not S16, no difference was observed during scrubbing.
[0071] Crystals also appear in juices S13 and S14, which contain an oil ratio of 20% and 50% respectively in the broad spectrum CBD / oil mixture, i.e., a proportion of 0.74% and 2.96% of the ES, respectively. The presence of these crystals is explained by the broad spectrum CBD being incorporated into the gum at a temperature below 60°C. For the amount of gum deposited to be regular and homogeneous, the juice must be free of suspended matter, as the latter could damage the gum juice delivery pump and plug the small diameter pipes between the pump and the nozzles. It is therefore necessary to heat the broad spectrum CBD to 60°C prior to its incorporation into the juice manufacturing reactor in the presence of all the additives.The amount of hemp oil in the ES is between 0% and 3% at 60°C minimum for the incorporation of broad spectrum CBD against more than 9% of hemp oil at room temperature for the incorporation of crystallized CBD with in both cases the same residual amount of CBD in the gum (2.52% of the ES).
[0072] Broad spectrum CBD is difficult to integrate into gum juice, but it appears much more appropriate to pre-mix the broad spectrum CBD with the additives sorbitol and possibly caramel and oil. The three-dimensional structure of the gum is more capable of trapping the broad spectrum CBD. It appears that for a high percentage of ES, candles / rises appear, whereas for lower ES (i.e. for a smaller quantity of gum added compared to the abundance of other additives, including broad spectrum CBD), these candles disappear. Analyses carried out with an infrared spectrometer on these candles have shown that they are essentially composed of CBD. Finally, it will also be possible to increase the quantity of broad spectrum CBD incorporated by also increasing the quantity of oil in the ES from 3% to 20%.Conversely, it is also possible to reduce the amount of oil used to solubilize the crystallized CBD by heating the enriched oil as well as the gum juice preparation reactor by double jacketing.
[0073] The graph of the figure 16 shows the results of tests carried out with different rubber mixtures: G1: Broad Spectrum CBD Blend, 100% Gum Arabic, 40.6% ES measured, 40.5% ES calculated, at 70°C and no caramel; G2: CBD-free Hemp Protein Blend with Hemp Protein, 100% Gum Arabic, 40.7% ES measured, 40.5% ES calculated, at 23°C; G3: CBD-free hemp protein blend with hemp protein, 100% gum arabic, 40.8% measured ES, 41% calculated ES, at 23°C G4: CBD-free blend, 98% gum arabic and 2% Karaya, 40.8% measured ES, 37.5% calculated ES, at 23°C G5: CBD-free blend, 80% gum arabic and 20% Cargill Icoat, 41% measured ES, 37.5% calculated ES, at 30°C
[0074] Hemp proteins are in the form of fine insoluble particles in the mixture, are visible in the gum and serve to give it a particular appearance. The amount of hemp proteins is preferably ≤ 3% of the ES.
[0075] We can see on the figure 16 that at 7 days the dynamic viscosity remains between 85 and 92 for all compositions G1 to G5.
[0076] It is found that at the levels of incorporation of the compounds of the preparation as described in the present application, the adhesiveness of the gum is not impacted by the addition of cannabinoids.
Claims
1. A gum of vegetable origin for rolling cigarette paper comprising a defined percent solids content, characterised in that it comprises a mixture of cannabinoids and edible oil, the edible oil being present in the mixture in a proportion p such that 0% ≤ p ≤ 80% by weight of the mixture, that the maximum amount of edible oil in the gum is limited to 20% by weight of the gum solids content, preferably less than 16% by weight of the gum solids content.
2. The gum according to claim 1, characterised in that the cannabinoid is crystallized cannabidiol (CBD) and that the edible oil is present in the mixture in a proportion p such that 20% ≤ p ≤ 80% by weight of the mixture.
3. The gum according to claim 1, characterised in that the cannabinoids are broad-spectrum cannabidiol (CBD) with or without oil and that the edible oil is present in the mixture with a proportion p such that 0% ≤ p ≤ 20% by weight of the mixture.
4. The gum according to one of the preceding claims, characterised in that the edible oil is hemp oil.
5. The gum according to one of the preceding claims, characterised in that it comprises an exudate of plants.
6. The gum according to the preceding claim, characterised in that the exudate is based on gum arabic.
7. The gum according to the preceding claim, characterised in that the gum arabic is comprised of 70% to 30% Senegal variety and 30% to 70% Seyal variety.
8. The gum according to claim 7, characterised in that gum arabic is comprised of 100% Seyal variety.
9. The gum according to claim 7, wherein gum arabic is comprised of 100% Senegal variety.
10. A rolling cigarette paper comprising gum according to one of the preceding claims.
11. The cigarette paper according to the preceding claim, characterised in that the gum is in the form of a trickle.
12. The cigarette paper according to claim 10, characterised in that the gum is in the form of a print.
13. A process for making a gum according to any one of claims 1 to 9, obtained from a gum juice and comprising the following steps of: - introducing a mixture of cannabinoid and edible oil in water, the edible oil being present in the mixture with a proportion p such that 0% ≤ p ≤ 80% by weight, - incorporating additives in the water, - dissolving and putting into solution in water a solids content composed of all the solids contained in the gum juice, - drying the gum juice.
14. The process according to the preceding claim, characterised in that the cannabinoid is oil-free, broad-spectrum cannabidiol (CBD) and in that it is heated to 70°C before introduction into the gum juice.
15. The process according to one of claims 13 or 14, characterised in that the gum juice is stirred and heated up to 70°C until the cannabinoid is fully diluted for homogeneous incorporation.
16. The process according to one of claims 13 to 15, characterised in that the gum juice has a dynamic viscosity at 22°C of between 65 seconds and 115 seconds, preferably between 85 and 92 seconds.
17. The process according to the preceding claim, characterised in that the gum juice comprises between 37% and 45% by weight of solids content.
18. The process according to one of the preceding claims, characterised in that the amount of exudate is greater than 75% by weight in the SC.