PL244559B1 - Method of producing modified jojoba oil and hardened wax - Google Patents

Abstract

The subject of the application is an innovative method for producing modified jojoba oil and hardened wax, in which the raw material jojoba oil, characterized by a cloud point of approx. 9°C, a pour point of approx. 8°C and a solidification point of approx. 7°C, is subjected to the process solvent separation into the filtrate - a solution of modified jojoba oil and the precipitate - hardened wax containing solvent residues, including a crystallization step and a filtration step, wherein in the crystallization step the raw material is first diluted with a solvent containing 10% - 100% (m/m) of methyl ethyl ketone and, respectively, 90% - 0% (m/m) of methyl tert-butyl ether, obtaining a mixture of raw material and solvent, which is then cooled at a controlled rate, with the simultaneous addition of the cooled solvent in 1-6 portions of subsequent dilution, with a cooling rate in the range of 0, 08 - 8.5°C/min until a temperature of -14 to -30°C is reached, with the ratio of the total amount of solvent from dilutions and washing to the raw material ranging from 1.4:1 to 9.8: 1 (m/m), where the size of each unit dilution expressed as the mass ratio of solvent to raw material is from 0.1:1 to 4.9:1 (m/m), and then in the temperature range from -14 to -30° C, the separated precipitate is filtered off and washed with a cold solvent of the same composition as the solvent used in the crystallization step, used in an amount from 0.15:1 to 6.0:1 (m/m), expressed as the mass ratio of the solvent to the raw material , and then the solvent is distilled from the filtrate to obtain the final product, which is modified jojoba oil with reduced: cloud point from 9 to 11°C, pour point from 9 to 13°C and solidification point from 9 to 13°C, and then with the solvent is distilled from the precipitate to obtain hardened wax with increased: cloud point from 6 to 9°C, pour point from 3 to 7°C and solidification point from 2 to 6°C in relation to the values of these temperatures before the raw material, jojoba oil, was subjected to the separation process solvent into the filtrate and precipitate and distilling the solvent from them.

Description

Description of the invention

The subject of the invention is a method for producing modified jojoba oil and hardened wax.

Modified wax, jojoba oil, thanks to its specific properties, can be used in many different industries - it can be used, for example, to produce lubricants, gear greases, high-pressure greases, heating oils, plasticizers and transformer oils. Hardened wax obtained from jojoba oil, thanks to its specific properties, will be used in many different industries, e.g. in cosmetics, pharmaceuticals, gear lubricants, high-pressure greases, heating oils, plasticizers, as a substitute for carnauba wax and beeswax.

Pro-ecological trends in many countries around the world result in the introduction of environmentally friendly products. Changes in the quality and type of manufactured products are stimulated by technical progress and efforts to reduce the negative impact on the environment and optimal use of raw material resources.

Actions to protect the natural environment require the adoption and application of all solutions in industrial processes aimed at reducing the negative effects related to the emission and use of harmful substances that degrade the natural environment. One of such solutions is the replacement of semi-finished products from crude oil processing, such as mineral base oils, slack waxes and paraffins, with natural waxes in technological processes.

The term "waxes" refers to a group of solid (organic) substances of natural or synthetic origin with a relatively low melting point and low viscosity in the liquid state. They are insoluble in water, have a melting point of up to 130°C and a density of 0.875-0.999 g/cm ³ (Mieczkowski P., Budziński B., "The influence of polyethylene wax on selected properties of asphalts and asphalt concretes"; Architectura 17 (4 ) 2018, 29-37; DOI: 10.22630/ASPA.2018.17.4.38).

Natural waxes can be divided into fossil waxes (e.g. lignite wax, ozokerite and macro and microcrystalline paraffin waxes) and non-fossil waxes. Non-fossil waxes are divided into waxes of animal origin (e.g. beeswax, shellac, lanolin, spermaceti) and waxes of plant origin (e.g. carnauba wax, candelilla wax, rice wax or jojoba oil) (Mieczkowski P., Budziński B., "The influence of polyethylene wax on selected properties of asphalts and asphalt concretes"; Architectura 17 (4) 2018, 29-37; Marszałek G., Majczak R., Polyethylene wax - preparation, modification and applications; POLIMERY 2012, 57, no. 9 640- 645).

The main components of non-fossil natural waxes are esters of fatty acids (so-called wax acids) and alcohols other than fats, i.e. glycerides (triglycerides of fatty acids). Waxes also contain free fatty acids, alcohols, hydrocarbons and their derivatives.

Jojoba oil is obtained from the crushed seeds of an evergreen, perennial desert shrub called Simonsidia Californian, found in the southwestern United States and northern Mexico. Jojoba oil contains about 50% (m/m) of an odorless, colorless oily liquid, which consists mainly of esters of C20-C24 monounsaturated fatty alcohols and C18-C22 monounsaturated fatty acids, it contains practically no glycerin, which makes jojoba oil fundamentally different from all known plant oils and is not a fat, but a liquid wax (Andreo-Martinez P., Garcia-Martinez N., Quesada-Medina J., RomanFigueroa C., PanequeM.; "Synthesis of value added fatty alcohols and FAMEs by non-catalytic supercritical methanol transesterification of jojoba (Simmondsia chinensis) wax"; Energy Conversion and Management 154 (2017) 430-439, Sanchez M., Avhad M. R., Marchetti J. M., Martinez M., Aracil J.; "Jojoba oil: A state of the art review and future prospects"; Energy Conversion and Management 129 (2016) 293-304; Apelblat A., Zaharoskin T., Wisniak I., Korngold E.; "Extraction of Oleic Acid from Soybean Oil and jojoba Oilm Phase Diagrams"; JAOCS, Vol. 73, no. 2).

Jojoba oil is a colorless, odorless, waxy liquid whose general structural formula is shown below:

CH3(CH2)nCH=CH(CH2)mCOO(CH2)jCH=CH(CH2)kCH3

PL 244559 Β1

Typical content of the main ingredients - acids and alcohols present in the form of esters in jojoba oil:

Fatty acids % mol Cl 8:1 8-15 C20:l 59-94 C22:l 10-15

Fatty alcohols % mol C20:l 40-46 C22:l 45-49 C24:l 6-10

Andreo-Martinez P., Garcia-Martinez N., Quesada-Medina J., Roman-Figueroa C., PanequeM.; "Synthesis of value added fatty alcohols and FAMEs by non-catalytic supercritical methanol transesterification of jojoba (Simmondsia chinensis) wax"; Energy Conversion and Management 154 (2017) 430^139.

As already mentioned, jojoba oil is a mixture of esters, which causes this specific wax to have a high dielectric constant and is susceptible to sulfurization and hydrogenation. Due to its specific properties, jojoba oil is used in many different industries, e.g. in the production of cosmetics, pharmaceuticals, lubricants, heating oils, transformer oils, plasticizers, flame retardants, foaming and anti-foaming agents, detergents, wetting agents and many others. Jojoba oil is also used as a substitute for carnauba wax and beeswax. (Shehata M.,S., Abdel Razek S., M., "Experimental investigation of diesel engine performance and emission characteristics using Jojoba/diesel blend and sunflower oil"; Fuel 2011; 90: 86-97; Turky G.M., El- Adly R.A., "Study of phase separation and anomalous molecular behavior of Jojoba oil using dielectric spectroscopy"; Journal of Molecular Liquids 242 (2017); Patent US4749517, "Ethoxylated jojoba oil"; ALCOLAC INC [US]; dated June 7, 19880) .

Mechanical pressing of jojoba oil seeds together with hexane extraction is a traditional method of obtaining jojoba oil and allows for increasing the oil yield between 3% and 8% m/m. The extraction process can only be carried out using organic solvents. Its main disadvantages are: a large amount of solvent used and a long process time, which makes it ineffective from an economic point of view and dangerous for the environment. Therefore, many efforts have been made to find cleaner methods of producing jojoba oil. One such method is the use of liquid carbon dioxide extraction under supercritical conditions, advantageous due to the advantages of CO2 as an inexpensive and completely inert solvent, however, the need to use high pressures makes this process still economically unattractive. For this reason, effective solutions are still being sought, e.g. the use of co-solvents such as ethanol or propane to increase the solubility of jojoba oil in CO2 (Sanchez M., Avhad M. R., Marchetti J. M., Martinez M., Aracil J.; Jojoba oil: "A State of the art review and future prospects”; Energy Conversion and Management 129 (2016) 293-304).

The authors of the article (Apelblat A., Zaharoskin T., Wisniak I., Korngold E.; "Extraction of Oil Acid from Soybean Oil and jojoba Oilm Phase Diagrams"; JAOCS, Vol. 73, no. 2) claim that traditionally used means extraction agents (mainly alcohols) for the separation of fatty acids from jojoba oil show rather low separation coefficients and selectivity, as well as high mutual miscibility with purified oil. The above publication describes a number of new solvents as potential fatty acid extractants. These solvents include: N-methylformamide, formamide, dimethylsulfoxide, 1,2-butanediol, and 2-butene-1,4-diol and 1,2-butanediol. Among the tested solvents, only N-methylformamide and 1,2-butanediol show desirable properties for the extraction of fatty acids from jojoba oil.

The patent application EP 2933322 describes a method for modifying animal and plant waxes, in particular beeswax and carnauba wax, consisting in limiting the amount of pesticides, in which the wax is mixed in a liquid state with a polar solvent heated to a temperature above the melting point of the wax for a specified time, and the mixture is then cooled to the point that the wax solidifies while the solvent remains liquid, and the solvent is then removed.

The polar solvent used is alcohol - ethanol or propanol or its isomers, and the wax is mixed with alcohol in a ratio of 20% wax to 80% alcohol and the mixture can, for example, be cooled to about 8°C.

The essence of the present invention is a method for producing modified jojoba oil and hardened wax, by subjecting the wax, jojoba oil, to a solvent separation process into the filtrate - a solution of modified jojoba oil and the precipitate - hardened wax containing solvent residues, based on the principles of the solvent dewaxing process, which is a process it is standardly used for dewaxing hydrocarbon oils and deoiling slack sludge - hydrocarbon mixtures. An important element of this classic process for hydrocarbon raw materials is the short filtration time, ranging from several to about 30 seconds; Moreover, a short filtration time allows to achieve a lower dewaxing temperature gradient, i.e. to achieve better selectivity of the process. Additionally, similar quality parameters of raw materials, i.e. jojoba oil and hydrocarbon feedstocks, such as viscosity, density, flash point, distillation range, allow the processing of jojoba oil in a solvent dewaxing installation without the need for modernization.

The process in question allows you to obtain a filtrate which, after distilling off the solvent, is modified jojoba oil, characterized by improved low-temperature properties, and a precipitate which, after removing the solvent, is hardened wax, i.e. the fraction remaining on the filter cloth, which after removing the solvent is characterized by increased temperature properties compared to for the load, raw jojoba oil.

The essence of the invention is a method for producing modified jojoba oil and hardened wax, by subjecting jojoba oil wax to a solvent separation process into the filtrate and precipitate of the raw material, and distilling the solvent from the filtrate and precipitate. This raw material, jojoba oil, contains chemical compounds other than the feedstocks consisting of various groups of hydrocarbons used in the classic dewaxing process, and feedstocks that are mixtures of fatty acid methyl esters (FAME) or triglycerides (fats).

Surprisingly, it turns out that the use of the solvent separation process into filtrate and sediment for jojoba oil maintains the selectivity of the process while obtaining short filtration times, which is desirable in industrial processes and allows for lowering the cloud point, pour point and solidification point, which affects the improving the low-temperature properties of the obtained product, modified jojoba oil and hardened wax, with increased parameters characterizing the temperature properties compared to the input.

According to the invention, the method for producing modified jojoba oil and hardened wax consists in the fact that the raw material jojoba oil, characterized by a cloud point of approximately 9°C, a pour point of approximately 8°C and a solidification point of approximately 7°C, is subjected to a separation process. solvent into the filtrate - a solution of modified jojoba oil and the precipitate - hardened wax containing solvent residues, including a crystallization step and a filtration step, wherein in the crystallization step the raw material is first diluted with a solvent containing 10%-100% (m/m) of methyl ethyl ketone and 90%, respectively %-0% (m/m) of methyl tert-butyl ether to obtain a mixture of raw material and solvent, which is then cooled at a controlled rate, with the simultaneous addition of the cooled solvent in 1-6 portions of successive dilution, with a solvent of the same composition as solvent used for the first dilution, at a cooling rate in the range of 0.08-8.5°C/min, until a temperature of -14 to -30°C is reached, with the ratio of the total amount of solvent from dilutions and washing to the raw material containing ranges from 1.4:1 to 9.8:1 (m/m), with the size of each unit dilution expressed as the mass ratio of solvent to raw material ranging from 0.1:1 to 4.9:1 (m/m). ), and then, in the temperature range from -14 to -30°C, the separated precipitate is filtered off and washed with a cold solvent of the same composition as the solvent used in the crystallization step, used in an amount from 0.15:1 to 6.0 :1 (m/m), expressed as the mass ratio of the solvent to the raw material, and then the solvent is distilled from the filtrate to obtain the final product, which is modified jojoba oil with reduced: cloud point, pour point and solidification point, and then the precipitate is distilled solvent, obtaining hardened wax with increased cloud point, pour point and solidification point in relation to the values of these temperatures before subjecting the raw material, jojoba oil, to the solvent separation process into the filtrate and precipitate and distilling the solvent from them.

Preferably, a crystallization modifier is additionally introduced into the raw material, containing polyalkyl methacrylates as an active substance, in an amount from 50 to 5000 ppm (mg/kg), most preferably 800-1200 ppm.

Waxes are polymorphic substances and additionally they tend to form much smaller crystals, creating spaces between the crystals in which the filtrate solution is trapped, which negatively affects the process of separating the filtrate solution from the sediment. The introduction of crystallization modifiers significantly improves filtration processes. In the present invention it has been found that polymeric substances of a similar type as used in the solvent dewaxing process, which favorably influence the crystallization process by promoting the formation of large regular crystals, despite the significant differences in chemical nature between waxes and hydrocarbons. Crystallization modifiers improve the speed and efficiency of the filtration process by influencing the structure of the sediment layer formed on the filter. Properly selected and used crystallization modifiers and chemical compounds specially developed for this purpose improve the efficiency and effectiveness of the entire dewaxing process. Crystallization modifiers used in solvent dewaxing processes are largely based on polyalkyl methacrylates (PAMA).

Preferably, the solvent used in the crystallization step and in the filtration step contains 35%-65% (m/m) methyl ethyl ketone and 65%-35% (m/m) methyl tert-butyl ether, respectively.

Preferably, the mixture is cooled at a rate of 0.2-1.8°C/min in the crystallization step. to temperature values from -24 to -28°C.

Preferably, the ratio of the total amount of solvent to raw material is in the range from 3.4:1 to 6.2:1 (m/m).

Preferably, the number of dilutions in the crystallization step is from 2 to 3.

Preferably, the separated esters are filtered off at temperatures ranging from -22 to -28°C and washed with a cold solvent used in an amount from 0.5:1 to 2.5:1.0 (m/m).

Preferably, in the crystallization step, the temperature of the solvent at the point of injection into the mixture is equal to or differs by a maximum of ± 3°C from the temperature of the cooled mixture. This is to prevent disruption of the crystallization process of esters in the mixture.

Preferably, in the crystallization step, the first portion of the solvent is introduced into the raw material at a temperature at which the raw material is a homogeneous liquid phase without crystals, most preferably at a temperature in the range of 35-60°C.

The modified jojoba oil produced by the method according to the invention is characterized by improved low-temperature properties, i.e. reduced cloud point, reduced pour point and reduced solidification point, in relation to the values of these temperatures before the jojoba oil was subjected to the solvent separation process. The modified jojoba oil produced by the method according to the invention can be used as a biodegradable base oil for the production of lubricants, gear greases, high-pressure greases, heating oils, plasticizers and transformer oils.

The hardened wax produced by the method according to the invention is characterized by increased temperature properties, i.e. increased cloud point, increased pour point and increased solidification point, in relation to the values of these temperatures before subjecting jojoba oil to the solvent separation process. Hardened wax obtained from jojoba oil, thanks to its specific properties, is used in many different industries, e.g. in cosmetics, pharmaceuticals, gear lubricants, high-pressure greases, heating oils, plasticizers, as a substitute for carnauba wax and beeswax.

The method according to the invention, consisting in using the process of solvent separation into the filtrate and precipitate for jojoba oil and distilling the solvent from them, gives the benefits of obtaining: a) one product - modified jojoba oil, characterized by improved low-temperature properties, i.e. reduced by several to approximately 13 degrees Celsius in terms of clouding, flow and solidification temperatures compared to the temperatures of the raw material used in the solvent separation process into filtrate and sediment, which translates into improved low-temperature properties, including rheological properties at low temperatures of the base oil, and provides the benefits of obtaining: b) the second product, hardened wax characterized by increased parameters characterizing temperature properties, i.e. increased by several to approximately 9 degrees Celsius clouding, flow and solidification temperatures compared to the temperatures of the raw material used in the process of solvent separation into filtrate and precipitate, which translates into obtaining higher freezing points for the final products in which they would be used

PL 244559 Β1 hardened wax instead of jojoba oil, and a positive pour point is desirable for these final products.

The subject matter of the invention is explained in the embodiments presented below, which do not limit the scope of its protection.

Example 1

Jojoba oil with the quality parameters presented in table 1 (marked OIL 1).

Table 1 Test results for jojoba oil (OIL 1)

No. Properties Unit Jojoba oil 1. Registration number - OIL 1 2. Kinematic viscosity at 40 °C ^mm2 /s 24.87 3. Kinematic viscosity at 100 °C mm ² ?s 6,509 4. Viscosity index - 237 5. Cloud point °c 9 6. Pour point °c 8 7. Solidification temperature °c 7 8. Oil content % m/m 14.86

A sample of jojoba oil (designated OIL 1) in the amount of 300 g was subjected to a solvent separation process into the filtrate and precipitate, using a mixture of methyl ethyl ketone (MEK) and methyl tert-butyl ether (MTBE) solvents.

Crystallization of wax (jojoba oil) in the laboratory was carried out by gradual cooling of the mixture of raw material and solvent contained in the crystallizer. The crystallizer was placed in a cooling bath equipped with a cooling cycle programmer, which allowed for determining the final crystallization temperature and the appropriate cooling rate in subsequent stages of the process. A filter cell equipped with a jacket in which the cooling medium circulates was connected to the cryostat.

The crystallization process was carried out using the dilution method, by adding subsequent portions of the cooled solvent to the cooled mixture of raw material and solvent at appropriate moments of the cooling cycle.

In the crystallization process, the contents of the crystallizer were continuously stirred using a mixer with an anchor tip, with the mixing speed adjusted to the increasing viscosity of the mixture.

After reaching the final crystallization temperature, the separated precipitate, the main component of which are glycerides - hardened waxes containing occluded solvent, was filtered from the filtrate solution using a vacuum filter. The filtrate solution accumulated in the receiver. The filtered precipitate was washed with a portion of cold solvent. The sediment collected from the nucha and the filtrate were subjected to the solvent distillation process to obtain the products, modified jojoba oil and hardened wax. The solvent removal operation was carried out by nitrogen stripping distillation.

Table 2 presents: technological parameters of the solvent separation process into filtrate and sediment, mass balance and properties of the obtained modified jojoba oil and hardened wax from jojoba oil.

PL 244559 Β1

Table 2 Technological parameters of the solvent separation process, mass balance and properties of the obtained modified jojoba oil and hardened wax from the raw material jojoba oil (OIL 1)

No dewaxing PR01 Type of solvent MEK-MTBE Technological parameters of the solvent separation process Solvent, mass ratio, MEK-MTBE 60:40 Crystallization/filtration temperature, °C -26 Total solvent to raw material ratio, (m/m) 5.5:1 Dilution T, tcmp.60°C, (m/m) 2.4 : 1 Dilution II, temp. -2 °C, (m/m) 2 : I Dilution III, temp.-l 1°C, (m/m) 0.5 : 1 Washing at filtration temperature, (m/m) 0.6 : 1 Mass balance of the solvent separation process Yield of modified jojoba oil, % (m/m) 28.0 Efficiency of hardened wax, % (m/m) 64.0 Losses, % (m/m) 8.0 sipping time, 22 sec a filter cake was formed Cooling time of the mixture from 60 °C to filtration temperature °C 1 hour 37 minutes Properties of modified jojoba oil Cloud point, °C -2 Pour point, °C -3 Freezing point, °C -4 Kinematic viscosity at 40 °C, mm ² /s 24.36 Kinematic viscosity at 100 °C, mm ² /s 6,259 Viscosity index 223 Oil content, % (m/m) 18.57 Properties of hardened wax Cloud point, °C 18 Pour point, °C 12 Freezing point, °C 10 Kinematic viscosity at 40 °C, mm ² /s 25.62 Kinematic viscosity at 100 °C, mm ² /s 6,581 Viscosity index 231 Oil content, % (m/m) 12/04

Example 2

A sample of jojoba oil (designated OIL 1) in the amount of 300 g was subjected to a solvent separation process into the filtrate and sediment, using a mixture of solvents: methyl ethyl ketone (MEK) and methyl tert-butyl ether (MTBE) according to the principles of procedure described in example 1.

Table 3 presents: technological parameters of the solvent separation process into filtrate and sediment, mass balance and properties of the obtained modified jojoba oil and hardened jojoba oil wax.

PL 244559 Β1

Table 3 Technological parameters of the solvent separation process, mass balance and properties of the obtained modified jojoba oil and hardened wax from the raw material jojoba oil (OIL 1)

No dewaxing PR 02 Type of solvent MEK-MTBE Technological parameters of the solvent separation process Solvent, mass ratio, MEK-MTBE 60:40 Crystallization/filtration temperature, °C -16 Total solvent to raw material ratio, (m/m) 6.5:1 Dilution I, temp.60°C, (m/m) 3.4 : 1 Dilution II, temp. -2 °C, (m/m) 2:1 Dilution III, temp.-l I°C, (m/m) 0.5 ; AND Washing at filtration temperature, (m/m) 0.6 : 1 Mass balance of the solvent separation process Yield of modified jojoba oil, % (m/m) 25.0 Efficiency of hardened wax, % (m/m) 66.5 Losses, % (m/m) 8.5 sipping time, 24 sec, a filter cake was formed Cooling time of the mixture from 60 °C to filtration temperature °C 1 hour 39 minutes Properties of modified jojoba oil Cloud point, °C -1 Pour point, °C -3 Freezing point, °C -4 Kinematic viscosity at 40 °C, mm7s 24.49 Kinematic viscosity at 100 °C, mm7s 6,258 Viscosity index 221 Oil content, % (m/m) 21.53 Properties of hardened wax Cloud point, C 15 Pour point, °C 12 Freezing point, °C 9 Kinematic viscosity at 40 °C, mm ² /s 25.69 Kinematic viscosity at 100 °C, mnr/s 6,587 Viscosity index 224 Oil content, % (m/m) 11.39

Example 3

A sample of jojoba oil (designated OIL 1) in the amount of 300 g was subjected to a solvent separation process into the filtrate and sediment, using a mixture of solvents: methyl ethyl ketone (MEK) and methyl tert-butyl ether (MTBE) according to the principles of procedure described in example 1.

Table 4 presents: technological parameters of the solvent separation process into filtrate and sediment, mass balance and properties of the obtained modified jojoba oil and hardened wax from jojoba oil.

PL 244559 Β1

Table 4 Technological parameters of the solvent separation process, mass balance and properties of the obtained modified jojoba oil and hardened wax from the raw material jojoba oil (OIL 1)

No dewaxing PR 03 Type of solvent MEK-MTBE Technological parameters of the solvent separation process Solvent» mass ratio, MEK-MTBE 80:20 Crystallization/filtration temperature, °C -16 Total solvent to raw material ratio, (m/m) 5.5:1 Dilution 1, temp. 60°C, (m/m) 2.4 : 1 Dilution II, temp. -2 °C, (m/m) 2:1 Dilution 111, temp. -8°C, (m/m) 0.5 : i Washing at filtration temperature» (m/m) 0.6 : I Mass balance of the solvent separation process Yield of modified jojoba oil, % (m/m) 28.9 Efficiency of hardened wax, % (m/m) 62.0 Losses, % (m/m) 8.1 sipping time, 21 sec a filter cake was formed Cooling time of the mixture from 60 C to filtration temperature °C 1 hour 24 minutes Properties of modified jojoba oil Cloud point, °C 0 Pour point, °C -1 Freezing point, °C -2 Freezing point, °C - Kinematic viscosity at 40 °C, mm ^! /p 24.51 Kinematic viscosity at 100 °C, mm7s 6,259 Viscosity index 221 Oil content, % (m/m) 20.74 Properties of hardened wax Cloud point, °C 17 Pour point, C 14 Freezing point, “C 12 Solidification point on the ball, °C - Kinematic viscosity at 40 °C, mnr/s 25.67 Kinematic viscosity at 100 °C, mirr/s 6,584 Viscosity index 223 Oil content, % (m/m) 12.27

Example 4

A sample of jojoba oil (designated OIL 1) in the amount of 300 g was subjected to a solvent separation process into the filtrate and sediment, using a mixture of methyl ethyl ketone (MEK) and methyl tert-butyl ether (MTBE) solvents according to the principles of procedure described in example 1, with the difference that that before

PL 244559 Β1 crystallization, a crystallization modifier was added to the raw material in an amount of 800 ppm with the trade name Viscoplex 9-327 containing from 15.0 to 40.0% (m/m) of the active substance - acrylic copolymers dissolved in mineral base oil, with viscosity at temperature 100°C 150 mm ² /s.

Table 5 presents: technological parameters of the solvent separation process into filtrate and sediment, mass balance and properties of the obtained modified jojoba oil and hardened wax from jojoba oil.

Table 5 Technological parameters of the solvent separation process, mass balance and properties of the obtained modified jojoba oil and hardened wax from the raw material jojoba oil (OIL 1)

No dewaxing PR 04 Type of solvent MEK-MTBE Viscosity modifier Viscoplex 9 - 327 (active substance: polyalkyl methacrylate) Technological parameters of the solvent separation process Solvent, mass ratio. MEK-MTBE 28:80 Crystallization/filtration temperature, °C -thirty Total solvent to raw material ratio, (m/m) 2.8:1 Dilution 1, temp. 60°C, (m/m) 2.3 : 1 Dilution II, temp. -2 ’C, (m/m) - 1 Dilution 111, temp.-H°C, (m/m) - Washing at filtration temperature, (m/m) 0.5 : 1 Mass balance of the solvent separation process Yield of modified jojoba oil, % (m/m) 29.4 Hardened wax yield, % (w/w} 59.3 Losses, % (m/m) 11.3 Sipping time. 15 seconds, a filter cake was formed Cooling time of the mixture from 60 "C to filtration temperature C 1 hour 58 minutes Properties of modified jojoba oil Cloud point, C -l Pour point, °C -3 Solidification temperature. C -4 Freezing point, °C - Kinematic viscosity at 40 ^C , mm7s 24.19 Kinematic viscosity at 100 °C, mm7s 6,273 Viscosity index 231 Oil content, % (m/m) 18.72 Properties of hardened wax Cloud point, “C 16 Pour point, "C 11 Freezing point, °C 10 Solidification point on the ball, °C - Kinematic viscosity at 40 °C, mA 25.61 Kinematic viscosity at 100 °C, iuif/s 6,658 Viscosity index 232 Oil content, % (m/m) 11.56

Example 5

A sample of jojoba oil (designated OIL 1) in the amount of 300 g was subjected to a solvent separation process into the filtrate and sediment, using a mixture of methyl ethyl ketone (MEK) and methyl tert-butyl ether (MTBE) solvents according to the principles of procedure described in example 1, with the difference that

PL 244559 Β1 that before crystallization, a crystallization modifier was added to the raw material in an amount of 2000 ppm with the trade name Viscoplex 9-350 containing the active substance - acrylic polymers dissolved in mineral base oil, with a viscosity at 100°C of 195 mm ² /s.

Table 6 presents: technological parameters of the solvent separation process into filtrate and sediment, mass balance and properties of the obtained modified jojoba oil and hardened wax from jojoba oil.

Table 6 Technological parameters of the solvent separation process, mass balance and properties of the obtained modified jojoba oil and hardened wax from the raw material jojoba oil (OIL 1)

No. deparaphmation PR 05 Type of solvent MEK-MTBE Viscosity modifier Vkcopłex 9 - 350 (subsL active alkyl polymethacrylate) Technological parameter of the solvent separation process Solvent, mass ratio, MEK-MTBE 90:10 Crystallization/filtration temperature, °C -25 Total solvent to raw material ratio, (m/m) 7.5:1 Dilution]. temp.°O^C, (m/m) 2.4 : 1 TL dilution temp. -2 °C, (m/m) 3 : 1 Dilution III, lamp -l 1°Q (m/m) 1.5 : 1 IV dilution, tcmp.-18 ^u C, (m/m) 0.6 : 1 Washing at filtration temperature, (m/m) 7.5:1 IWims bulk solvent separation process Efficiency of modified jojoba oil, % (m/m) 32.4 Efficiency of hardened wax, % (m/m) 58.9 Losses, % (/«4«) «,7 Sipping time. 9 sec, a filter cake was formed Cooling time of the mixture from 60 'C to filtration temperature °C 1 hour 57 minutes Properties of modified jojoba oil Cloud point, ^U C -2 Pour point, °C -5 Freezing point, ^l1 C -6 Kinematic viscosity at 40 °C, mm ^? /p 24/07 Kinematic viscosity at 100 °C, i/s 6,252 Viscosity index 231 Oil content, % (w/w) 19.53 Properties of hardened wax Cloud point, “C 16 Pour point, ^dC 15 Freezing point, C 13 Kinematic viscosity at 40 °C, mm'/s 25.68 Kinematic viscosity at IOO°C, 6,676 Viscosity index 232 Oil content, % (/«//Ml 8.45

PL 244559 Β1

Example 6

A sample of jojoba oil (marked OIL 1) in the amount of 300 g was subjected to a solvent separation process into the filtrate and sediment using the solvent methyl ethyl ketone (MEK) according to the principles of procedure described in example 1.

Table 7 presents: technological parameters of the solvent separation process into filtrate and sediment, mass balance and properties of the obtained modified jojoba oil and hardened wax from jojoba oil.

Table 7 Technological parameters of the solvent separation process, mass balance and properties of the obtained modified jojoba oil and hardened wax from the raw material jojoba oil (OIL 1)

No dewaxing PR 06 Type of solvent MEK Technological parameters of the solvent separation process Solvent, mass ratio, MEK - Crystallization/filtration temperature, °C -25 Total solvent to raw material ratio, (m/m) 5.5:1 Dilution I, temp.60°C, (m/m) 2.4 : 1 Dilution Π, temp. -2 °C, (m/m) 2:1 Dilution III, tcmp.-l 1°C, (m/m) 0.5 : 1 IV dilution, temp. -18°C, (m/m) Washing at filtration temperature, (m/m) 0.6 : 1 Mass balance of the solvent separation process Performance of modified jojoba oil. % (m/m) 21.5 Efficiency of hardened wax, % (m/m) 70.1 Losses, % (m/m) 8.4 sipping time, 6 sec, a filter cake was formed Cooling time of the mixture from 60 °C to filtration temperature 'C 1 hour 24 minutes Properties of modified jojoba oil Cloud point, ^O C Pour point, °C -3 Freezing point, °C -4 Kinematic viscosity at 40 °C, mm ² /s 24.47 Kinematic viscosity at 100 °C, mnr/s 6,278 Viscosity index 224 Oil content, % (m/m) 22.41 Properties of arilized wax Cloud point, 'C 14 Pour point, 'C 11 Freezing point, C 9 Kinematic viscosity at 40 °C, mm ³ /s 25.54 Kinematic viscosity in I00 “C, mm’/s 6,663 Viscosity index 232 Oil content, % 12.46

Claims (9)

1. A method for producing modified jojoba oil and hardened wax, characterized in that the raw material jojoba oil, characterized by a cloud point of approximately 9°C, a pour point of approximately 8°C and a solidification point of approximately 7°C, is subjected to a solvent separation process into the filtrate - a solution of modified jojoba oil and the precipitate - hardened wax containing solvent residues, including a crystallization stage and a filtration stage, where in the crystallization stage the raw material is first diluted with a solvent containing 10%-100% (m/m) of methyl ethyl ketone and 90%, respectively -0% (m/m) of methyl tert-butyl ether to obtain a mixture of raw material and solvent, which is then cooled at a controlled rate, while simultaneously adding the cooled solvent in 1-6 portions of subsequent dilution, with a solvent of the same composition as the solvent used for the first dilution, at a cooling rate in the range of 0.08-8.5°C/min., until a temperature of -14 to -30°C is reached, with the ratio of the total amount of solvent from dilutions and washing to the raw material being in the range from 1.4:1 to 9.8:1 (m/m), with the size of each unit dilution expressed as the mass ratio of solvent to raw material ranging from 0.1:1 to 4.9:1 (m/m) , then, in the temperature range from -14 to -30°C, the separated precipitate is filtered off and washed with a cold solvent of the same composition as the solvent used in the crystallization step, used in an amount from 0.15:1 to 6.0: 1 (m/m), expressed as the mass ratio of the solvent to the raw material, and then the solvent is distilled from the filtrate, obtaining the final product, which is modified jojoba oil with reduced: cloud point, pour point and solidification point, and then the solvent is distilled from the precipitate, obtaining hardened wax with increased: cloud point, pour point and solidification point in relation to the values of these temperatures before subjecting the raw material, jojoba oil, to the process of solvent separation into filtrate and precipitate and distilling the solvent from them. 2. The method according to claim 1, characterized in that a crystallization modifier is additionally introduced into the raw material, containing polyalkyl methacrylates as an active substance, in an amount from 50 to 5000 ppm (mg/kg), preferably 800-1200 ppm. 3. The method according to claim 1 or 2, characterized in that the solvent used in the crystallization step and in the filtration step contains 35%-65% (m/m) methyl ethyl ketone and, respectively, 65%-35% (m/m) methyl tert-butyl ether 4. The method according to claim 1 or 2 or 3, characterized in that the mixture is cooled at a rate of 0.2-1.8°C/min in the crystallization step. to temperature values from -24 to -28°C. 5. The method according to claim 1. 1 or 2 or 3, characterized in that the ratio of the total amount of solvent to the input is in the range from 3.4:1 to 6.2:1 (m/m). 6. The method according to claim 1. 1 or 2 or 3, characterized in that the number of dilutions in the crystallization step is from 2 to 3. 7. The method according to claim 1. 1 or 2 or 3, characterized in that the separated precipitate is filtered in the temperature range from -22 to -28°C and washed with a cold solvent used in an amount from 0.5:1 to 2.5:1.0 (m/ m). 8. The method according to claim 1 or 2 or 3, characterized in that in the crystallization step the temperature of the solvent at the point of injection into the mixture is equal to or differs by a maximum of ± 3°C from the temperature of the cooled mixture. 9. The method according to claim 1. 1 or 2 or 3, characterized in that in the crystallization step the first portion of the solvent is introduced into the raw material at a temperature at which the raw material is a homogeneous liquid phase not containing crystals, preferably in the range of 35-60°C.