JPS598390B2 - Oil and fat refining method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for refining fats and oils, and more particularly to a method for obtaining refined fats and oils with excellent color and stability.

The usual refining of fats and oils involves a degumming process using mineral or organic acids, followed by a deacidification process consisting of neutralizing free fatty acids with an alkaline aqueous solution and washing the resulting soap with warm water. Next, it goes through a number of steps, including a decolorization process using adsorbents such as activated clay and activated carbon, and a deodorization process using steam under vacuum.

However, the quality of oils and fats refined using these conventional refining methods, such as hue, storage stability, and thermal stability, is inconsistent, so it is necessary to increase the amount of adsorbent added or change the type of adsorbent in the decolorization process. In many cases, it is necessary to do this, and even if you do this, there are cases where you cannot obtain refined oils and fats of good quality. This is mainly due to the quality of the raw material oil and fat.

In other words, differences in hue, acid value, peroxide value, carbonyl value, impurity content, etc. occur due to differences in the collection method, storage method, period, transportation method, etc. of raw material fats and oils. This has led to variations in the quality of refined oils and fats.
The present invention is an improvement on the conventional refining method that has such drawbacks, and is a refining method that can always obtain refined oils and fats of excellent quality even if the quality of the raw material oils and fats varies.

That is, the present invention is characterized in that, in addition to the known method for refining fats and oils, before the deodorizing step, a step is performed in which the fats and oils are brought into contact with an acidic sulfite compound and an inorganic phosphoric acid compound at the same time, and then insoluble matter is removed. This is a method of refining fats and oils.

The contact treatment step using the acidic sulfite compound and the inorganic phosphoric acid compound of the present invention can be performed before each step such as a degumming step, a deoxidizing step, and a decoloring step, or simultaneously with each of these steps.

In particular, it is preferable to carry out the treatment before the degumming step or the decoloring step, or at the same time as these steps. Before the degumming process,
Alternatively, if the contact treatment step of the present invention is performed at the same time as the degumming step, by carefully performing the next deoxidizing step, a refined fat or oil of such a light color that the decoloring step can be omitted can be obtained.

When acidic sulfite compounds and inorganic phosphoric acid compounds are brought into contact with fats and oils at the same time, oxidation products such as peroxides and carbonyl compounds, gums, and other impurities contained in the fats and oils are converted into reduced stable compounds and It is thought that it changes into a compound that is easily removed. The contact treatment conditions in the present invention are that an acidic sulfite compound and an inorganic phosphoric acid compound are added at the same time in an amount of 0.01 to 5% by weight, respectively, to the fat and oil, and
The contact is carried out at 150°C for 2 to 90 minutes.

The fats and oils to which the present invention is applicable include beef tallow, pork fat, fish oil,
There are animal oils and fats such as whale oil, vegetable oils and fats such as palm oil, soybean oil, cottonseed oil, linseed oil, olive oil, perilla oil, castor oil, rapeseed oil, and rice bran oil.In addition to synthetic glycerides, there are also various carboxylic acids and various alcohols. It can also be applied to the purification of esters.

Examples of acidic sulfite compounds used in the present invention include sulfurous acid, acidic ammonium sulfite, acidic sodium sulfite, acidic potassium sulfite, acidic calcium sulfite, nitrile hydrogen sulfite, and ethyl hydrogen sulfite.

Inorganic phosphoric acid compounds include phosphoric acid, phosphorous acid, hypophosphorous acid, monoammonium phosphate, diammonium phosphate,
Triammonium phosphate, monosodium phosphate, disodium phosphate, trisodium phosphate, monopotassium phosphate,
Dipotassium phosphate, tripotassium phosphate, monocalcium phosphate, dicalcium phosphate, tricalcium phosphate, sodium pyrophosphate, potassium pyrophosphate, sodium acid pyrophosphate, potassium acid pyrophosphate, sodium polyphosphate, potassium polyphosphate , Sodium Metaphosphate, Potassium Metaphosphate, Magnesium Acid Phosphate, Dilithium Acid Phosphate, Barium Acid Phosphate, Ammonium Phosphite, Sodium Phosphite, Potassium Phosphite, Calcium Phosphite, Sodium Hypophosphite, These include potassium phosphite, calcium hypophosphite, and aluminum hypophosphite.

Next, the present invention will be explained with reference to Examples and Comparative Examples.

Note that % indicates weight %. In addition, the analytical values of refined oils and fats of each example and comparative example and the AOM test (AOCS test method Cd
Table 1 shows the peroxide values for 12-57), and the refined fats and oils obtained by the method of the present invention have a better hue compared to the refined fats and oils obtained by the conventional method, and exhibit excellent stability in the AOM test. That is clear.

Example Palm oil heated to 180°C (acid value 0.7, iodine 53.0, peroxide value 6.0, hue too reddish-orange to measure) was mixed with 75% phosphoric acid 1% and acidic ammonium sulfite 0. After adding 5% and stirring for 30 minutes, insoluble matter was removed by centrifugation.

Next, add 3.0% (1.5 times equivalent to the acid value of palm oil) of a caustic soda aqueous solution of 4-maro porta and heat at 80℃ for 50 minutes.
After stirring for several minutes, the produced liquid was removed by centrifugation, and washed with warm water until the washing liquid showed neutrality.

After dehydrating under vacuum, add 1% activated clay and incubate at 140℃ for 3 hours.
After stirring for 0 minutes and filtering off the activated clay at 100℃, 5 m
7! Steam deodorization was performed at LHgl260°C for 90 minutes. Comparative Example 1 To the same palm oil as in Example 1 heated to 80°C, 1% of 75% phosphoric acid was added, stirred for 30 minutes, and then centrifuged to remove insoluble matter.

Next, deoxidizing, decolorizing, and deodorizing steps were performed in the same manner as in Example 1.

Comparative Example 2 To the same palm oil as in Example 1 heated to 80° C., 3% of 75% phosphoric acid was added, stirred for 30 minutes, and then centrifuged to remove insoluble matter.

Next, deoxidizing, decolorizing, and deodorizing steps were performed in the same manner as in Example 1.

Comparative Example 3 3% acidic ammonium sulfite was added to the same palm oil as in Example 1 heated to 80° C., stirred for 30 minutes, and then centrifuged to remove insoluble matter.

Next, deoxidizing, decolorizing, and deodorizing steps were performed in the same manner as in Example 1.

Example 2 To the same palm oil as in Example 1 heated to 80°C, 0.1% of 20% diluted sulfuric acid was added and stirred for 5 minutes, and then the precipitate and diluted sulfuric acid were centrifuged.

Next, acidic sodium sulfite and calcium hypophosphite?
After adding 1% of each and stirring at 90° C. for 30 minutes and centrifuging insoluble matter, deoxidizing, decolorizing and deodorizing steps were performed in the same manner as in Example 1. Comparative Example 4 Purification was carried out under exactly the same conditions as in Example 2, except that the contact treatment with acidic sodium sulfite and calcium hypophosphite was not performed.

Comparative Example 5 Purification was carried out under exactly the same conditions as in Example 2, except that 3% calcium hypophosphite was used instead of the contact treatment with acidic sodium sulfite and calcium hypophosphite.

Comparative Example 6 Example 2 except that the contact treatment was performed using 3% sodium acid sulfite instead of the contact treatment with sodium acid sulfite and calcium hypophosphite.
Purification was carried out under exactly the same conditions.

Example: To the same palm oil as in Example 1 heated to 380°C, 0.5% each of acidic calcium sulfite and potassium pyrophosphate were added, stirred for 60 minutes, and then centrifuged to remove insoluble matter. The deoxidizing, decolorizing, and deodorizing steps were performed in the same manner as in 1.

Comparative Example 7 Purification was carried out under exactly the same conditions as in Example 3, except that the contact treatment using acidic calcium sulfite and potassium pyrophosphate was not performed.

Comparative Example 8 Purification was carried out under exactly the same conditions as in Example 3 except that 3% potassium pyrophosphate was used instead of the contact treatment with acidic calcium sulfite and potassium pyrophosphate.

Comparative Example 9 Purification was carried out under exactly the same conditions as in Example 3, except that instead of the contact treatment with acidic calcium sulfite and potassium pyrophosphate, 3% of acidic calcium sulfite was used for the contact treatment.

Example 3% ethyl hydrogen sulfite and 1% lithium hydrogen phosphate were added to the same palm oil as in Example 1 heated to 480°C, stirred for 30 minutes, and then centrifuged to remove insoluble matter.

Next, 1% phosphoric acid was added and the mixture was stirred at 80° C. for 30 minutes, followed by centrifugation to remove insoluble matter. Next, Example 1
The deoxidizing, decolorizing, and deodorizing steps were carried out in the same manner as above. Example 5 0.2% phosphoric acid was added to the same palm oil as in Example 1 heated to 80° C., and after stirring for 30 minutes, insoluble matter was removed by centrifugation.

Then, after performing a deoxidizing step in the same manner as in Example 1, acidic sodium sulfite and monoammonium phosphate were each reduced to zero.
．． 2% was added and stirred at 90°C for 10 minutes. Next, 2% of activated clay was added and stirred at 140°C for 30 minutes.
After cooling to 0.degree. C., filtration was performed.

Furthermore, a deodorizing step was performed in the same manner as in Example 1. Example 6
Beef tallow heated to 80℃ (acid value 5.7, iodine value 46.5
, peroxide value 15.0, hue: Lovibond R5.6, Y
4O [5-inch cell]), 1% phosphoric acid and 2 sulfite water
% and stirred for 30 minutes, the insoluble matter was centrifuged.

Next, a 4.3% aqueous solution of caustic soda at 20 degrees Celsius was added and stirred for 5 minutes, and the resulting liquid was centrifuged. After washing with water and dehydrating in the same manner as in Example 1, 2% of activated clay was added and stirred at 100°C for 30 minutes. The beef tallow obtained by filtering this was heated to 511Hg and 240°C.
Steam deodorization was performed for 60 minutes. Comparative Example 10 Beef tallow was purified under exactly the same conditions as in Example 6, except that sulfite water was not used.

Comparative Example 11 In Example 6, except that the contact treatment was performed using 5% phosphoric acid instead of the contact treatment with phosphoric acid and sulfite water.
Purification was carried out under exactly the same conditions.

Comparative Example 12 Purification was carried out under exactly the same conditions as in Example 6, except that instead of the contact treatment with phosphoric acid and sulfite water, 5% sulfite water was used for the contact treatment.

Example 7 To the same beef tallow as in Example 6 heated to 80°C, 3% each of acidic ammonium sulfite and ammonium phosphite were added and stirred for 20 minutes.

After centrifuging the insoluble matter, deacidification, decolorization, and deodorization steps were performed in the same manner as in Example 6. Comparative Example 13 Purification was carried out under exactly the same conditions as in Example 7, except that the contact treatment with acidic ammonium sulfite and ammonium phosphite was not performed.

Comparative Example 14 In Example 7, instead of the contact treatment with acidic ammonium sulfite and ammonium phosphite,
Purification was carried out under exactly the same conditions except that the contact treatment was carried out using 7% ammonium phosphite.

Comparative Example 15 In Example 7, instead of the contact treatment with acidic ammonium sulfite and ammonium phosphite,
Purification was carried out under exactly the same conditions except that the contact treatment was carried out using 7% acidic ammonium sulfite.

Example 8 Purification was carried out under the same conditions as in Example 7, except that sodium acid sulfite and sodium metaphosphate were used at 2.5% each in place of acidic ammonium sulfite and ammonium phosphite.

Example 9 An esterification reaction was carried out at 220 to 240°C for 10 hours using glycerino 184f (2 mol), oleic acid 1708t (6.1 mol) and zinc oxide 19r.

The obtained oleic acid triglyceride had an acid value of 9.7. Add 1% each of acidic sodium sulfite and calcium hypophosphite to this oleic acid triglyceride at 80°C.
and stirred for 30 minutes.

After centrifuging the insoluble matter, add a 7.2% caustic soda aqueous solution (1.5% to the acid value of the ester) boiled at 20 degrees.
5 times equivalent) and stirred for 5 minutes. Next, the separated portion was centrifuged, washed with warm water, and then dehydrated under vacuum. After adding 2% activated clay and stirring at 120°C for 30 minutes, filtration was performed at 100°C, and then 57 nm
Steam deodorization was performed with Hg at 1250°C for 60 minutes. Comparative example
16 Purification was carried out under exactly the same conditions as in Example 9, except that the contact treatment with acidic sodium sulfite and calcium hypophosphite was not performed.

Comparative Example 17 Purification was carried out under exactly the same conditions as in Example 9, except that 3% calcium hypophosphite was used instead of the contact treatment with acidic sodium sulfite and calcium hypophosphite.

Comparative Example 18 Purification was carried out under exactly the same conditions as in Example 9, except that instead of the contact treatment with sodium acid sulfite and calcium hypophosphite, 3% sodium acid sulfite was used for the contact treatment.

Claims (1)

[Claims] 1. In addition to the usual method for refining fats and oils, the method is characterized by carrying out a step of simultaneously bringing an acidic sulfite compound and an inorganic phosphoric acid compound into contact with the fat and oil before the deodorizing step, and then removing insoluble matter. A method for refining fats and oils. 2. The method for refining fats and oils according to claim 1, wherein the step of simultaneously contacting the fats and oils with an acidic sulfite compound and an inorganic phosphoric acid compound and then removing insoluble matter is performed before the deacidification step.