EP3247780B1

EP3247780B1 - Palm oil product for use as a candle wax and process

Info

Publication number: EP3247780B1
Application number: EP15817233.8A
Authority: EP
Inventors: Krishnadath Bhaggan; Mariska HOLWEDEL; Hang Kam MAN
Original assignee: Bunge Loders Croklaan BV
Current assignee: Bunge Loders Croklaan BV
Priority date: 2014-12-23
Filing date: 2015-12-17
Publication date: 2019-02-20
Anticipated expiration: 2035-12-17
Also published as: PL3247780T3; WO2016102318A1; EP3247780A1

Description

This invention relates to a palm oil product for use as candle wax, and a process for manufacturing such a palm oil product.
Traditionally, paraffin wax is a preferred material used as candle wax, allowing for candles with good burning properties and attractive visual appearance. Currently, palm based fats are used to replace (part of) paraffin in the production of candles. The main palm products that are used are palm oil (PO), hydrogenated palm oil (PO60) and palm stearin (e.g., palm oil stearin having an iodine value of (IV) of 35; POsIV35). These palm products need to be used in specific blend ratios in order to obtain the required characteristics (e.g. melting point, crystallization behavior) needed for candles.
Palm oil is usually processed in order to obtain products having specific properties. For example, palm oil may be fractionated to separate the higher melting components, usually referred to as palm stearin, from the lower melting components, usually referred to as palm olein. The composition of the fractions depends on the conditions under which fractionation is carried out.
Fractionation of palm oil is generally carried out by one of three methods i.e., dry fractionation, solvent fractionation and fractionation in the presence of a detergent. In dry fractionation, the stearin is crystallized from the oil in the absence of a solvent using temperature to control the formation of solids as crystals. Solvent fractionation involves the addition of solvents such as acetone to effect the separation of the stearin from the olein.
The problem the industry is facing when applying palm oil products in candles is sweating. Sweating is defined as the formation of liquid oil droplets occurring at the surface of the candle material during storage at room temperature (20°C). The rate of sweating may be increased at elevated temperatures. Such elevated temperatures may occur during storage, in particular in warm countries or close to heat-generating apparatuses. The occurrence of sweating causes an unappealing appearance of the candle surface, and may deposit oils on packaging materials as well as dirtying the hands of users when touching the candle surface.
WO03012016 describes a candle which does not contain paraffin wax or any other petroleum based product. Instead the candles described in this application contain vegetable oils as a primary component. The examples included candles formed from 80-100 wt. % of palm stearin blended with 0-20 wt. % hydrogenated palm oil.
WO2007136259 describes a method of manufacturing a candle comprising a vegetable oil, having at least 10 wt. % of a palm oil fraction with a melting point of 32-54 C, blended with a further combustible material selected from the group consisting of petroleum-based wax, fatty acid, bees wax and combinations thereof; and at least 10 wt. % of hydrogenated oil.
EP1693436 describes fully hardened or partially hardened triglyceride vegetable oil compositions that are mentioned for a number of uses including emulsifiers, fatty acids, softeners, detergents and waxes (candles). The hardened oil may be derived from palm nut oil, palm oil, palm oil oleins, palm oil stearines, palm oil mid fractions, olive oil, rapeseed oil, canola oil, linseed oil, ground nut oil, soybean oil, cotton seed oil, sunflower seed oil, pumpkin seed oil, coconut oil, corn oil, castor oil, walnut oil, hazelnut oil, safflower oil, false flax oil and mixture/s thereof. The patent description does not indicate any specific compositions.
There remains a need for a palm oil product for use as candle wax, which is easy to produce. In particular, there is a desire for such a palm oil product having no sweating or a reduced sweating. It would be even more desirable if such a palm oil product would have a smooth surface appearance.
According to the present invention, a palm oil product for use as candle wax is provided, wherein the palm oil product consists of partially hydrogenated palm olein, wherein the partially hydrogenated palm olein comprises a mono unsaturated fatty acids (MUFA) content from 15 to 25 wt. %.
Such products are easy to produce, by partially hydrogenation of palm olein until the required MUFA content is acquired. It was found that these products do not display significant sweating. In addition, these products have a smooth surface appearance.
The term "fatty acid", as used herein, refers to saturated or unsaturated, straight chain carboxylic acids having from 8 to 24 carbon atoms. Unsaturated acids may comprise one, two, or more double bonds, preferably one or two double bonds.
Fatty acids are predominantly covalently bonded in glycerides in the palm oil products. Thus, the fatty acid content of a glyceride composition includes the fatty acids present in mono-, di- and tri- glycerides. The total fatty acid content of a composition may be determined by FAME analysis.
The fatty acid compositions are characterized in the content of saturated fatty acids (SAFA), monounsaturated fatty acids (MUFA) and polyunsaturated fatty acids (PUFA). Mono unsaturated fatty acids (MUFA) are fatty acids having a single carbon-carbon double bond, which may be in either the cis or trans configuration. The group of MUFA includes but is not restricted to palmitoleic acid (C16:1 cis) and oleic acid (C18:1 cis). As defined herein, MUFA is the total of C16:1 c/t, C18:1 c/t, C20:1 c/t, C22:1 c/t and C24:1 c/t; wherein c/t indicates the combined amounts of cis and trans fatty acids for that particular number of carbon atoms. Polyunsaturated fatty acids (PUFA) have more than one carbon-carbon double bond, such as two or three double bonds.
It is preferred if the partially hydrogenated palm olein comprises MUFA from 18 to 25 wt. %. Throughout this specification, percentages of fatty acids are by weight based on total fatty acid content.
In an aspect of the invention, the partially hydrogenated palm olein has a fatty acid composition comprising at least 70 wt. % saturated fatty acids (SAFA) and from 15-25 wt. % monounsaturated fatty acids MUFA; wherein SAFA and MUFA amount up to a total of at least 90 wt. % of the total fatty acid composition, preferably at least 95 wt. %.
SAFA are fatty acids without unsaturated bonds, such as palmitic acid (C16:0) and oleic acid (C18:0). As defined herein, SAFA is the total of C12:0, C14:0, C16:0, C17:0, C18:0, C20:0, C22:0 C24:0.
In another aspect of the invention, it is preferred if the fatty acids composition of the partially hydrogenated palm olein comprises from 35-45 wt. % palmitic acid (C16:0); and from 25-40 wt. % stearic acid (C18:0); and wherein palmitic acid and stearic acid together make up for at least 70 wt. % of the fatty acids composition. Preferably, palmitic acid and stearic acid together make up for at least 90 wt. % of the SAFA fraction of the total fatty acids composition.
In another aspect of the invention, the MUFA consists of at least 95 wt. % of C18 monounsaturated fatty acids, preferably at least 99 wt. %.
In yet another aspect of the invention, the partially hydrogenated palm olein has a saturated fatty acid (SAFA) to mono-unsaturated fatty acid (MUFA) weight ratio of 2-5, preferably 2.5-4.
In an aspect of the invention, the partially hydrogenated palm olein has a Mettler Dropping Point (MDP) value above 52 °C, as determined according to AOCS Cc 18-80.
In another aspect of the invention, the partially hydrogenated palm olein has an iodine value (IV) of from 18-30, as calculated according to AOCS Cd 1c-85, based on the fatty acid composition, determined using fatty acid methyl ester analysis (FAME) gas chromatography according to ISO 15304.
In yet another aspect of the invention, the palm oil product is shaped as a candle, and the palm oil product is provided with a wick. Optionally, the palm product can be provided with one or more candle wax additives, including but not limited to: candle dyes or colorants; fragrances; fragrance binding agents; particles for visual effects; UV stabilizers.
The invention further provides a process for the manufacture of a palm oil product as described in claim 1 for use in candles comprising the steps of: providing a palm olein fraction having a mono unsaturated fatty acids (MUFA) content of at least 30 wt. %, and partially hydrogenating of the palm olein fraction to produce a partially hydrogenated palm oil olein having a mono unsaturated fatty acids (MUFA) content from 15 to 25 wt. %.
In an aspect of the invention, the partially hydrogenated palm olein has a fatty acid composition comprising from 35-45 wt. % palmitic acid (C16:0); from 25-40 wt. % stearic acid (C18:0); and from 15-25 wt. % mono unsaturated fatty acids MUFA; wherein palmitic acid and stearic acid are present in a combined amount up to at least 70 wt. % of the fatty acid composition, and wherein C16:0, C18:0 and MUFA amount up to a total of at least 90 wt. % of the total fatty acid composition, preferably at least 95 wt. %.
The partially hydrogenated palm olein is obtained without further blending with other vegetable oils and/or mineral oils, in particular not with paraffin and/or palm stearin. The partially hydrogenated palm olein as described herein can be shaped into candles. Optionally, the palm product as described may be subjected to standard refining before manufacturing candles.
Also disclosed is the use of a palm oil product as a candle wax, wherein the palm oil product essentially consists of partially hydrogenated palm olein, wherein the partially hydrogenated palm olein comprises a mono unsaturated fatty acids (MUFA) content from 15 to 25 wt. %, for example to reduce sweating and/or to improve surface appearance. The palm oil product is preferably a palm oil product of the invention.
The invention will now be further elucidated according to the following non-limiting examples.

EXAMPLES

Example 1

A palm oil product suitable for use as a candle wax substitute was prepared by partial hydrogenation. The product thus obtained was suitable for use as a candle wax without further blending, and did not show sweating in the sweat test as described herein.

Preparation

1500 gram of palm olein having an iodine value of 56 and a MUFA content of 43 wt. % was put in a lab scale autoclave and heated to 180-190°C. This oil was partially hydrogenated by adding about 56L of hydrogen gas at a pressure of 2 bar, which reaction was catalyzed by a nickel catalyst. The palm olein was partially hydrogenated to an iodine value of between 19 and 23, and a total MUFA content of between 19 wt. % to 24 wt. %. After the reaction, the catalyst was filtered off and the oil was further refined according to standard procedures.
The experiment was repeated for samples A and B, with a degree of hydrogenation up to IV 24 and 21, respectively. For comparison, a comparative sample COMP was also prepared according to the same procedure as A and B, with a lower degree of hydrogenation up to IV 37, having a significantly higher amount of MUFA compared to samples A and B.
For further comparison in the analysis, a blend of palm oil (PO) and PO60 (fully hydrogenated palm oil, IV<1) was taken, which is commercially used as a candle wax substitute. This blend is labelled herein as PO/PO60.
Additional samples used for comparison are the non-hardened palm stearin fractions POs IV35 and POs IV14, as well as the fully hydrogenated palm oil PO60. POs IV35 has a relatively high MUFA content, POs IV14 has a relatively low MUFA content. The fully hydrogenated palm oil PO60 is essentially free of unsaturated fatty acids, and would therefore have a MUFA <1 wt. %.

Analysis

Analytical data is shown in table 1. MDP is the Mettler Dropping Point, as determined according to AOCS Cc 18-80. IV was determined by calculation according to AOCS Cd 1c-85 from the fatty acid composition analysis (IV FAME). The fatty acid composition analysis (FAME) was determined using gas chromatography according to ISO 15304, for C8:0, C10:0, C12:0, C14:0, C16:0, C17:0, C18:0, C18:1 c/t, C18:2 c/t, C18:3 c/t, C20:0, C20:1 c/t, C20:2 c/t, C22:0 , C22:1 c/t, C24:0, C24:1 c/t. The label c or t indicates the cis and trans isomers of the respective fatty acid.

The fatty acid compositions are further characterized in terms of their content of saturated fatty acids (SAFA), monounsaturated fatty acids (MUFA) and polyunsaturated fatty acids (PUFA). For the purpose of this study, MUFA is the total of C16:1c/t, C18:1 c/t, C20:1 c/t, C22:1 c/t and C24:1 c/t; SAFA is the total of C8:0, C10:0, C12:0, C14:0, C16:0, C17:0, C18:0, C20:0, C22:0 C24:0; and PUFA is the total of C18:2 c/t, C18:3 c/t, C20:2 c/t as determined in percentage by weight (wt. %). From these numbers, the SAFA/MUFA ratio can be calculated.

Table 1: Analytical data.

	COMP	A	B	PO/PO60	POs IV35	POs IV14	PO60
Analysis
MDP	50.4	56.1	57.0	55.2	55.2	62.2	61.8
IVFAME	37.2	24.0	21.0	34.2	33.0	13.3	0.7

C8:0	0.0	0.0	0.0	0.0	0.0	0.0	0.0
C10:0	0.0	0.0	0.0	0.0	0.0	0.0	0.0
C12:0	0.2	0.2	0.2	0.1	0.3	0.3	0.4
C14:0	1.0	1.0	1.0	1.2	1.2	1.3	1.3
C15:0	0.1	0.0	0.1	0.1	0.1	0.1	0.1
C16:0	40.1	40.0	40.5	59.9	49.7	80.0	58.9
C16:1T	0.1	0.0	0.0	0.0	0.0	0.0	0.0
C16:1C	0.1	0.0	0.0	0.1	0.1	0.1	0.0
C17:0	0.1	0.1	0.1	0.1	0.1	0.1	0.1
C18:0	16.2	32.0	34.8	4.8	16.3	4.8	37.9
C18:1	39.7	23.7	20.4	26.6	25.2	10.6	0.5
C18:1T	28.1	14.6	12.5	0.1	0.0	0.0	0.0
C18:1C	11.6	9.2	7.9	26.5	25.2	10.6	0.5
C18:2	1.6	2.0	1.9	6.2	6.2	2.3	0.1
C18:2T	1.6	2.0	1.9	0.2	0.1	0.1	0.0
C18:2C	0.1	0.0	0.0	6.1	6.1	2.2	0.1
C18:3	0.1	0.0	0.0	0.1	0.1	0.1	0.0
C18:3T	0.0	0.0	0.0	0.0	0.0	0.0	0.0
C18:3C	0.0	0.0	0.0	0.1	0.1	0.0	0.0
C20:0	0.4	0.5	0.5	0.3	0.4	0.3	0.5
C20:1C	0.0	0.0	0.0	0.1	0.1	0.0	0.0
C20:2C	0.0	0.0	0.0	0.0	0.0	0.0	0.0
C22:0	0.1	0.1	0.1	0.1	0.1	0.1	0.1
C22:1	0.0	0.0	0.0	0.0	0.0	0.0	0.0
C22:1T	0.0	0.0	0.0	0.0	0.0	0.0	0.0
C22:1C	0.0	0.0	0.0	0.0	0.0	0.0	0.0
C24:0	0.1	0.1	0.1	0.1	0.0	0.1	0.1
C24:1C	0.0	0.0	0.0	0.0	0.0	0.0	0.0
Unidentified	0.2	0.3	0.4	0.1	0.1	0.0	0.0

SAFA	58.3	73.9	77.2	66.8	68.1	87.0	99.3
MUFA	39.8	23.7	20.5	26.8	25.4	10.7	0.5
PUFA	1.7	2.0	1.9	6.4	6.4	2.4	0.1

Ratio SAFA/MUFA	1.46	3.11	3.77	2.49	2.68	8.13	191.02

Sweating test

The samples listed in table 1 were heated to 60°C, poured into candle-shaped moulds, and provided with a wick to form a candle. In this case, the moulds were tea light cups, but other shaped moulds could be used. The moulds were cooled to room temperature (about 20°C) and when totally solidified, the moulds were transferred to a cabinet with pre-set controlled temperature at 40°C.

The candles were visually inspected for sweating behaviour after about 18 hrs. A detailed view for samples COMP, A and B is shown in figure 1. Figure 2 shows top views of the samples prior to the sweating test, whereas figure 3 shows the same samples after 18 hours of storage at 40°C. The samples were assessed for sweating behaviour, the smoothness of the surface, and the general surface appearance. Results of the sweat test are summarized in table 2, as judged by an experienced test panel.

Table 2: Qualitative evaluation of sweat test results.

	COMP	A	B	PO/PO60	POs IV35	POs IV14	PO60
Sweating	+	-	-	-	-	-	-

Surface Smoothness	+	++	++	+	-	--	-

Appearance	Liquid oil visible	Matte	Matte	Glossy	Soft, dull	Hard, irregular surface	Hard, cracks

The presence of liquid oil droplets at the surface indicates sweating in the COMP sample, as clearly shown. Both the sample A with a MUFA content of 22 wt. % and B with a MUFA content of 20 wt. % did not show any sweating. The commercially used PO/PO60 blend also does not show significant sweating, but has the disadvantage that it needs an additional blending step to manufacture compared to A and B.
In addition, both A and B show a visually attractive surface. Both samples A and B have a smooth surface. The commercially used PO/PO60 tends to form more irregularities. A as well as B further display a pleasant matte surface finish, in contrast to the commercially used PO/PO60 which has a glossy appearance. For some types of candles, a matte surface finish is preferred over a glossy surface. Samples A and B achieve a matte surface finish without post processing of the candle.
The samples POs IV35, POs IV14 and PO60 also do not show sweating, but are unsuitable as a regular candle wax substitute. POs IV35 is too soft to retain its shape without further support. POs IV14 has a very hard structure and tends to form an unattractive, irregular surface due to its crystalline properties. PO60 also has a very hard structure, and tends to form unattractive cracks on the surface.

Claims

Palm oil product for use as candle wax, wherein the palm oil product consists of partially hydrogenated palm olein, wherein
the partially hydrogenated palm olein comprises a mono unsaturated fatty acids (MUFA) content from 15 to 25 wt. %.
Palm oil product according to claim 1, wherein the partially hydrogenated palm olein comprises MUFA from 18 to 25 wt. %.
Palm oil product according to claim 1 or 2, wherein the partially hydrogenated palm olein has a fatty acid composition comprising
at least 70 wt. % saturated fatty acids (SAFA) and
from 15-25 wt. % monounsaturated fatty acids MUFA;
wherein SAFA and MUFA amount up to a total of at least 90 wt. % of the total fatty acid composition, preferably at least 95 wt. %.
Palm oil product according to claim 3, wherein the fatty acids composition of the partially hydrogenated palm olein comprises
from 35-45 wt. % palmitic acid (C16:0); and
from 25-40 wt. % stearic acid (C18:0); and
wherein palmitic acid and stearic acid together make up for at least 70 wt. % of the fatty acids composition.
Palm oil product according to any of the preceding claims, wherein the MUFA consists of at least 95 wt. % of C18 monounsaturated fatty acids, preferably at least 99 wt. %.
Palm oil product according to any of the preceding claims, wherein the partially hydrogenated palm olein has a saturated fatty acid (SAFA) to mono-unsaturated fatty acid (MUFA) weight ratio of 2-5, preferably 2.5-4.
Palm oil product according to any of the preceding claims, wherein the partially hydrogenated palm olein has a Mettler Dropping Point (MDP) value above 52°C, as determined according to AOCS Cc 18-80.
Palm oil product according to any of the preceding claims, wherein the partially hydrogenated palm olein has an iodine value (IV) of from 18-30, calculated according to AOCS Cd 1c-85, based on the fatty acid composition, determined using fatty acid methyl ester analysis (FAME) gas chromatography according to ISO 15304.
Palm oil product according to any of the preceding claims, wherein the palm oil product is shaped as a candle, and wherein the palm oil product is provided with a wick, and optionally provided with one or more candle wax additives, including but not limited to: candle dyes or colorants; fragrances; fragrance binding agents; particles for visual effects; UV stabilizers.
Process for the manufacture of a palm oil product according to any of the preceding claims for use in candles, comprising the steps of:
- providing a palm olein fraction having a mono unsaturated fatty acids (MUFA) content of at least 30 wt. %, and

- partially hydrogenating of the palm olein fraction to produce a partially hydrogenated palm olein having a mono unsaturated fatty acids (MUFA) content from 15 to 25 wt. %.
Process according to claim 10, wherein the partially hydrogenated palm olein has a fatty acid composition comprising
from 35-45 wt. % palmitic acid (C16:0);
from 25-40 wt. % stearic acid (C18:0); and
from 15-25 wt. % monounsaturated fatty acids MUFA;
wherein palmitic acid and stearic acid are present in a combined amount up to at least 70 wt. % of the fatty acid composition, and wherein C16:0, C18:0 and MUFA amount up to a total of at least 90 wt.% of the total fatty acid composition, preferably at least 95 wt.%.