RU2086616C1 - Method for producing lipids and wax - Google Patents

Abstract

FIELD: fat-and-oil and perfume-cosmetic industries. SUBSTANCE: ground bark of coniferous trees are extracted by hydrocarbon solvent. Extract is boiled down up to concentration of dry substances 6-10%. Precipitated wax is filtered, washed by hydrocarbon solvent, and dried. Residue of solvent is eliminated from concentrate, while volatile terepene compositions are removed by direct steam. EFFECT: higher efficiency. 2 tbl

Description

 The invention relates to the perfumery and cosmetics industry, specifically to the production of lipids and wax for cosmetics from the bark of coniferous trees.

 Lipids are substances that are found in living organisms. This definition includes a large number of compounds, including higher hydrocarbons, alcohols, aldehydes, fatty acids, carotenoids, sterols, fat-soluble vitamins, waxes.

 Waxes are esters of fatty acids and fatty alcohols, fatty acids and sterols.

 It is known that wax and lipids are widely used as intermediates for cosmetic products. The currently used raw materials for wax and lipids / beeswax, pink wax, spermaceti / hard to reach. Attracting new sources of raw materials in the production of these products is an urgent task. The use of bark of coniferous trees as a source of waste from the timber industry complex will make it possible to obtain them on a large scale.

 To extract lipids from plant tissues, the Blyay and Dyer method is used, including grinding of plant materials, extraction with a mixture of chloroform-methanol / 1: 2 / under ordinary conditions, hydromodule 7, the extract is filtered, a mixture of chloroform and water is added to it, then organic and aqueous the layers are separated, benzene is added to the chloroform layer and concentrated in vacuo. In other cases, isopropanol, ethanol, benzene, or mixtures of organic solvents are used as lipid extractant. However, the use of complex extracting mixtures requires a complex technology for their subsequent separation, the methanol present in the mixture creates a danger in operation.

 There is another method for extracting lipids from the bark of coniferous trees with gasoline.

 The authors of this method do not give the quality of the obtained lipids, since the purpose of the invention was to increase the yield of tannic extracts, which was achieved by preliminary extraction of hydrophobic components (lipids) and this improved the conditions for the extraction of hydrophilic components (tannins) with water. Thus, lipids were a by-product in the description of the process, but may suggest that the lipids obtained by this method in their composition contain gasoline, monoterpene hydrocarbons and alcohols, which give an unpleasant tarry odor, so this product cannot be used in the cosmetic industry.

The closest technical solution, selected as a prototype, is a method for producing lipids and wax from coniferous greenery by chopping greenery, extracting it with BR-1 gasoline at a temperature of 80 ^o C, the duration of the extract is 5.5 6 hours. After the extraction is completed , the extract is pumped to the settlers, where waxy products precipitate. Duration of wax deposition is 24 hours. After wax deposition, the gasoline extract is filtered and sent to a distillation cube, where gas is distilled from fat-soluble substances (lipids), first with blank steam, and then, sharp steam is fed into the distillation cube to remove tail gas fractions and essential oils. . The distillation is continued until traces of oil in the distillation appear.

 VAT residue of fat-soluble substances (lipids) is used to obtain chlorophyll-carotene paste.

 The technology for obtaining coniferous wax is as follows. Once every 5 days, the sumps are cleaned of waxy substances deposited on the wall. To do this, sharp steam is supplied to the sump and the waxy substances in molten form are sent to a distillation cube for gas distillation. After distillation of gasoline, the melt is hot filtered from mechanical impurities, poured into molds and sent to the finished goods warehouse. The specified method has disadvantages.

1. The method does not allow to obtain lipids as a commodity product, but only as raw materials for further processing, since according to the technology used, light essential oils with a density of 0.815-0.875 g / cm ³ and a refractive index of n are distilled from lipids $\genfrac{}{}{0ex}{}{\text{twenty}}{\text{d}}$ 1.4640-1.4720. These indicators indicate that the composition of essential oils includes terpene hydrocarbons (α-pinene, Δ ³ karen, dipentene), and terpineol. High boiling terpene compounds (sesquiterpenes, alcohols) with a density of more than 0.875 g / cm ³ and n $\genfrac{}{}{0ex}{}{\text{twenty}}{\text{d}}$ 1.4930 and more remain in lipids, give the product a sharp tarry odor and limit their scope in cosmetics.

2. The technology for producing wax has a number of negative aspects:
firstly, this process can only be periodic, and therefore energy-intensive;
secondly, waxing is carried out from a low-concentration solution (0.3% solution of wax in gasoline), i.e. the solution is in the metastable region (the region of unsaturated solutions. As you know, the boundaries of the metastable region depend on the cooling rate, evaporation and other factors. With a relatively small decrease in temperature (as in the prototype), the system slowly passes into the labile region of the supersaturated solution, where the solid phase is released This process is multi-stage and takes place in time. In the prototype, the wax is extracted 126 hours from the moment the woody greens are processed;
thirdly, the duration of the process dramatically reduces the utilization of equipment.

fourthly, repeated contact of wax with a periodically drained, fresh lipid extract leads to a significant accumulation of chlorophyll, carotene, their derivatives and other lipid components in wax, which leads to a deterioration in the quality of wax and limited use in cosmetics;
Fifthly, wax cleaning is carried out by filtration only from mechanical impurities, which is an insufficient measure to obtain a high-quality product that does not contain chlorophyll and carotene derivatives.

 The purpose of the invention: obtaining high-quality intermediates for cosmetic products from the bark of coniferous trees: lipids, wax.

This goal is achieved by the fact that:
The crust is crushed, extracted with a hydrocarbon solvent, the extract is evaporated to a non-volatile content 6-10% solution is cooled to a temperature of 15-20 ^o C, the precipitated wax is filtered off, washed with a non-polar hydrocarbon solvent, dried. The solvent is distilled off from the filtrate, and the residual solvent and high boiling terpene compounds are distilled off with sharp steam.

Distinctive features of the method are:
1. The use of bark of coniferous trees as a source of raw materials for semi-products of the cosmetic industry.

 2. Separation of high-boiling terpene compounds by steam stripping.

 3. Deposition of wax from a pre-concentrated and chilled lipid extract.

 The proposed method is illustrated by the following examples.

Example 1. 50 g of crushed (2-10 mm) larch bark with a moisture content of 10%, which contains 3% lipids and wax, is loaded into the extractor with 280 g of Nefras A 65/75 gasoline (hydraulic module 1: 5.6). The extraction is carried out at a temperature of 65 ^o C for 3 hours. The extract is filtered off from suspended particles and evaporated at a temperature of 65 ^o C to a dry matter concentration of 6%, cooled to a temperature of 15 ^o C. In the resulting concentrate, wax precipitates, which is filtered and washed with Nefras gasoline A 65/75 The wax is dried, and the washing filtrates are combined, the solvent is distilled off, raising the temperature in the mass to 102 ^° C, then the volatile components are distilled off with a sharp steam at a temperature of 120 ^° C. The yield of wax is 0.13 g (0.30% of a.s. cortex). The yield (of lipids) is 0.174 g (2.6% of the a.s. of the cortex). Total recovery rate 96.6%
The resulting lipids have the following indicators:
acid number 90 mg KOH / g
ether number 30 mg KOH / g
bromine number 80 mg Br / g,
hydroxyl number 100 mg KOH / g
dropping point 45-50 ^o C.

Received wax has the following indicators:
acid chill 55 mg KOH / g
ether number 95 mg KOH / g
bromine number 40 mg Br / g,
hydroxyl number 210 mg KOH / g
dropping point 65-75 ^o C.

The yield of volatile high-boiling terpene hydrocarbons is 0.02 g (0.04% to a.s. to). Density d 0.910 g / cm ³ .

Example 2. 50 g of chopped (2-10 mm) spruce bark with a moisture content of 10%, which contains 4.0% lipids and wax, is charged with Nefras A 65/75 gasoline in an amount of 210 g (hydromodule 4.2). The extraction is carried out at a temperature of 65 ^o C for 2 hours. The extract is filtered off from suspended particles, cow dust and the solvent is distilled off at a temperature of 65 ^o C to a solids concentration of 8% in the extract is cooled to a temperature of 18 ^o C.

Wax precipitates in the resulting concentrate, which is filtered off and washed with Nefras A 65/75 gasoline. The wax is dried, and the washing filtrates are combined, the solvent is distilled off, raising the temperature to 102 ^o C, then with the help of sharp steam the volatile components are distilled off at a temperature of 130 ^o C.

The lipid yield of 1.583 g (3.4% of the A.C. of the cortex). The yield of wax is 0.19 g (0.42% of the a.s. of the bark). Total recovery rate 96%
The resulting lipids have the following characteristic:
acid number 74.5 mg KOH / g
ether number 53.0 mg KOH / g
bromine number 83.6 mg Br / g,
hydroxyl number 74.5 mg KOH / g,
dropping point 34-40 ^o C.

The resulting wax has the following characteristics:
acid number 57.5 mg KOH / g
ether number 56.2 KOH / g
bromine number 68.4 mg Br / g,
hydroxyl number 178.5 mg KOH / g,
dropping point above 200 ^o C.

The yield of volatile high-boiling terpene compounds is 0.02 g (0.05% of a.s. to.) With a density of 0.900 g / cm ³ .

Example 3. The extractor is loaded with 50 g of crushed (2-10 mm) pine bark with a moisture content of 10% which contains 4.5% lipids and wax, quenched with Nefras A 65/75 gasoline in an amount of 400 g (hydraulic unit 1: 8). The extraction is carried out at a temperature of 65 ^o C for 4 hours. The extract is filtered off from suspended particles of cow dust and the solvent is distilled off at a temperature of 65 ^o C until the solids concentration in the extractor is 10%, cooled to a temperature of 20 ^o C. In the resulting extract, wax is precipitated, which is filtered and washed with Nefras A 65/75 gasoline. The wax is dried, and the washing filtrates are combined, the solvent is distilled off, raising the temperature in the mass to 102 ^° C, then the volatile components are distilled off with a sharp steam at a temperature of 140 ^° C until the tar smell is removed.

The lipid yield is 1.8 g (4.0% of the A.C. of the cortex). The yield of wax is 0.16 g (0.36% of the a.s. of the bark). Total recovery rate 96.6%
The resulting lipids have the following indicators:
acid number 60.0 mg KOH / g
ether number 60.0 mg KOH / g
bromine number 55.0 mg Br / g,
hydroxyl number 55.0 mg KOH / g,
dropping point 45.0 ^o C
Received wax has the following indicators:
acid number 92.0 mg KOH / g,
ether number 61.1 mg KOH / g
hydroxyl number 160 mg Br / g.

The yield of volatile high-boiling terpene compounds is 0.027 g (0.06% a.s.c.) with a density of 0.897 g / cm ³ . A comparison of the process parameters of the proposed method and the prototype are presented in table 1
The quality of lipids and wax is presented in table.2.

 The research institute of synthetic and natural aromatic substances (VNIISNDV) tested lipids and wax.

 From the test results it follows that lipids and wax obtained from the bark of trees of various conifers are high-quality intermediates for the products of the perfumery and cosmetics industry: toothpastes, shampoos.

Thus, the proposed method will allow:
1. Improve the quality of wax compared with the prototype, since the proposed method purifies the wax from chlorophyll and its derivatives by washing with a hydrocarbon solvent.

 2. To simplify the process of obtaining wax and increase the utilization rate of equipment by 15 times compared with the prototype, this eliminates the many-hour stage of sedimentation of lipids and the multi-day stage of collecting wax.

 3. To expand the raw material base in comparison with analogues and the range of products of the perfumery and cosmetics industry.

 4. To increase the utilization rate of coniferous biomass by 2–4.5%, since at present the tree bark is a multi-ton waste of the timber processing industry.

 The proposed method for the production of lipids and wax from the bark of coniferous trees was mastered at the TsNILKH Experimental Plant; industrial implementation is offered at enterprises that process coniferous wood.

Claims (1)

A method of producing lipids and wax by extraction of plant materials with a non-polar hydrocarbon solvent, evaporation of the extract, separation of wax and distillation of the solvent, volatile with steam, characterized in that the bark of coniferous trees are extracted, the extract is evaporated to a dry matter concentration of 6 10% concentrated solution is cooled to 15 20 ^o C, the precipitated wax is filtered off, washed with a non-polar hydrocarbon solvent, dried, and the filtrate is evaporated, residual solvent and volatile impurities are distilled off with steam.

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