WO2016142953A2 - Procédé de purification de cires - Google Patents

Procédé de purification de cires Download PDF

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Publication number
WO2016142953A2
WO2016142953A2 PCT/IN2016/000060 IN2016000060W WO2016142953A2 WO 2016142953 A2 WO2016142953 A2 WO 2016142953A2 IN 2016000060 W IN2016000060 W IN 2016000060W WO 2016142953 A2 WO2016142953 A2 WO 2016142953A2
Authority
WO
WIPO (PCT)
Prior art keywords
wax
ethanol
mixture
refluxing
crystallised
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/IN2016/000060
Other languages
English (en)
Other versions
WO2016142953A3 (fr
Inventor
Mangehs Ganesh KULKARNI
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Praj Industries Ltd
Original Assignee
Praj Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Praj Industries Ltd filed Critical Praj Industries Ltd
Priority to JP2017548218A priority Critical patent/JP7150434B2/ja
Publication of WO2016142953A2 publication Critical patent/WO2016142953A2/fr
Publication of WO2016142953A3 publication Critical patent/WO2016142953A3/fr
Priority to PH12017501626A priority patent/PH12017501626A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/12—Refining fats or fatty oils by distillation
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

Definitions

  • the invention relates to a method for the purification of crude rice bran and sunflower waxes using an alcohol as a purifying solvent. It particularly relates to the use of ethyl alcohol as said solvent for efficient and economic purification of crude rice bran and sunflower waxes into economically valuable high purity wax products.
  • Rice is one of the most important grains in the world and India is second largest producer of it.
  • the rice bran is a valuable by-product of rice milling industry. It is recently used for prepare edible rice bran oil as a valuable product.
  • the bran contains about 12% to 25% oil component.
  • Beside oil, the bran also contains about 5% waxy materials called rice bran wax, which is by-product of rice bran oil refining process.
  • the crude wax has certain low value applications; however if purified to certain higher degree it forms a valuable product as being used in cosmetics and food preparations.
  • the rice bran wax is a heterogeneous product with made up of saturated monoesters of long chain fatty acid [C-22 to C-26] and long chain fatty alcohols [C-26 to C-30] . Up on refining or purification the wax becomes a relatively homogenous mixture having physical characters like melting point of about 78 ° C to 82 °C , saponification value of about 70 to 120 units and iodine value of about 4 to TO units.
  • This purified rice bran wax then has many industrial applications like leather polishes, crayons, candles, shoe creams, paper coatings, carbon papers, lubricants etc. Other major applications are in food industry like in chocolate enrobes, vegetable coatings and wax emulsions for fruit preservation. It is further used in pharmaceuticals products like tablets, ointments, suppositories and cosmetic products like moisturizing lotions, lipsticks, skin creams etc.
  • the rice bran wax is purified or refined is by removing the residual oil from it by hydraulic pressing to maximum extent possible, followed by extracting it in- solvents like isobutanol or isopropanol with water.
  • these extractions are costly for recycling of isobutanol or isopropanol in the process is expensive and efficiency of the process is limited.
  • the disclosed invention describes a novel method of purification of crude rice bran wax to high purity waxes.
  • the disclosure provides a method for purifying crude rice bran wax comprising: mixing said wax with ethanol forming a mixture; refluxing said mixture for a desired time dissolving said wax; allowing said mixture to stand idle for desired time; separating undissolved matters from liquid fraction; cooling said liquid fraction allowing formation of crystallised wax; removing said crystallised wax by filtration; washing said crystallised wax by ethanol; repeating steps above up to four times with said undissolved matters to extract remaining wax; and pooling and drying said crystallised wax under vacuum forming a final product that is a purified rice bran wax with consistent characters of physical and chemical properties
  • the disclosure provides a method for purifying crude sunflower wax comprising: mixing said wax with ethanol forming a mixture; refluxing said mixture for a desired time dissolving said wax; allowing said mixture to stand idle for desired time; separating undissolved matters from liquid fraction; cooling said liquid fraction allowing formation of crystallised wax; removing said crystallised wax by filtration; washing said crystallised wax by ethanol; repeating steps above up to three times with said undissolved matters to extract remaining wax; and pooling and drying said crystallised wax under vacuum forming a final product that is a purified sunflower wax with consistent characters of physical and chemical properties
  • the crude rice bran wax obtained as a by-product of rice bran oil refining process is dissolved in absolute ethyl alcohol.
  • the wax is refluxed at about 75 °C in a reflux vessel for about 1 hour to allow dissolution of rice bran wax into ethanol leaving resinous impurities undissolved in the mixture.
  • the oil present in the crude is also dissolved in ethanol.
  • the . liquid fraction is decanted and allowed to cool to room temperature for the wax to crystallize out from the solution.
  • the solid wax is removed by filtration under vacuum, one washed with ethanol, optionally decoloured with an oxidizing agent, and dried to get the white to pale yellow solid mass of purified rice bran wax having consistent physical and chemical properties like melting temperature and purity.
  • the resinous matters obtained are further subject to ethanol refluxing to recover remaining wax up to 4 times, if required.
  • the crude rice bran wax contains up to 50% oil, which is obtained as a by-product of the process disclosed herein. Further remaining resinous matters may also be as crude waxy material.
  • the crude sunflower wax obtained as a byproduct of the sunflower oil refining process is dissolved in absolute ethyl alcohol.
  • the wax is refluxed at about 75 ° C in a reflux vessel for about 1 hour to allow dissolution of said wax into ethanol leaving impurities undissolved in the mixture.
  • the oil present in the crude is also dissolved in ethanol.
  • the liquid fraction is decanted and allowed to cool to room temperature for the wax to crystallize out from the solution.
  • the solid wax is removed by filtration under vacuum, once washed with ethanol, optionally decoloured with an oxidizing agent, and dried to get the white to pale yellow solid mass of purified sunflower wax having consistent physical and chemical properties like melting temperature and purity.
  • the impurities/ residues obtained are further subject to ethanol refluxing to recover remaining wax up to 3 times, if required.
  • the crude sunflower wax contains up to 40% oil, which is obtained as a byproduct of the process disclosed herein. Further remaining residues may also be as crude waxy material.
  • ethanol used as the solvent for refluxing of the crude rice bran or sunflower wax is absolute ethanol or ethanol at least 99% pure by volume. Any reduction in the purity of ethanol below 99% leads to drastic reduction in the final yield of purified said waxes as the presence of water in ethanol leads to reduction in the dissolution of waxes in ethanol.
  • the refluxing of said waxes and ethanol mixture is performed for at least one hour at temperature about 75 °C with an efficient condenser to prevent loss of the solvent.
  • the said purified waxes are used in preparation of pharmaceutical or cosmetic products that required unique characters of the wax like its melting temperature, texture, colour, etc.
  • said liquid fraction pool was cooled at room temperatiire, allowed to stand idle for dissolved wax to crystallize out from oil and other impurities, and then separated by vacuum filtration. Said crystallized wax was once washed with about product [purified rice bran wax]. These steps afforded about 48 g of highly pure final wax product with acid value of about 1.5 units, saponification value of about 87 units and iodine value of about 27 units with white to white colour. This product has a melting point of about 80 °C. Further, about 37 g of oil and about 8 g of solid impurities were recovered as byproducts.
  • said liquid fraction pool was cooled at 10 °C temperature, allowed to stand idle for dissolved wax to crystallize out from oil and other impurities, and then separated by vacuum filtration.
  • Said crystallized wax was once washed with about 100 mL of ethanol and dried under vacuum to form the final wax product [purified rice bran wax].
  • These steps afforded about 31 g of highly pure final wax product with acid value of about 2 units, saponification value of about 71 units and iodine value of about 30 units with white to white colour.
  • This product has a melting point of about 78 °C.
  • about 33 g of oil and about 33 g of solid product were recovered as byproducts.

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Fats And Perfumes (AREA)
  • General Preparation And Processing Of Foods (AREA)

Abstract

La présente invention concerne un procédé de purification de cires de son de riz et de tournesol brutes à l'aide d'un alcool en tant que solvant de purification. Elle concerne en particulier l'utilisation d'alcool éthylique en tant que solvant pour une purification efficace et économique de cires de son de riz et de tournesol brutes, ce qui permet d'obtenir des cires extrêmement pures intéressantes sur le plan économique.
PCT/IN2016/000060 2015-03-10 2016-03-03 Procédé de purification de cires Ceased WO2016142953A2 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2017548218A JP7150434B2 (ja) 2015-03-10 2016-03-03 ロウの精製のための方法
PH12017501626A PH12017501626A1 (en) 2015-03-10 2017-09-07 Method for the purification of waxes

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
IN780/MUM/2015 2015-03-10
IN780MU2015 2015-03-10
IN201621007004 2016-02-29
IN201621007004 2016-02-29

Publications (2)

Publication Number Publication Date
WO2016142953A2 true WO2016142953A2 (fr) 2016-09-15
WO2016142953A3 WO2016142953A3 (fr) 2016-10-27

Family

ID=56879953

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IN2016/000060 Ceased WO2016142953A2 (fr) 2015-03-10 2016-03-03 Procédé de purification de cires

Country Status (3)

Country Link
JP (1) JP7150434B2 (fr)
PH (1) PH12017501626A1 (fr)
WO (1) WO2016142953A2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019097535A1 (fr) * 2017-11-20 2019-05-23 Praj Industries Limited Purification de cires à haute pression
CN110607204A (zh) * 2019-10-29 2019-12-24 江苏京晶光电科技有限公司 一种从蓝宝石贴片废料中对液态蜡回收方法

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60155143A (ja) * 1984-01-24 1985-08-15 Nippon Oil & Fats Co Ltd 天然ロウからの脂肪族高級アルコ−ルの分離法
JPS60188305A (ja) * 1984-03-07 1985-09-25 Nisshin Oil Mills Ltd:The 化粧料
JPH06200289A (ja) * 1992-12-28 1994-07-19 Nippon Petrochem Co Ltd 天然粗ワックスの精製方法
JPH0711285A (ja) * 1993-06-25 1995-01-13 Nisshin Oil Mills Ltd:The 植物ワックスの精製法
AUPO605097A0 (en) * 1997-04-07 1997-05-01 James Cook University Of North Queensland Food grade wax and process for preparing same
JP4125532B2 (ja) * 2002-03-28 2008-07-30 カウンシル・オブ・サイエンティフィック・アンド・インダストリアル・リサーチ 粗米ぬかワックスの品質改良および漂白方法および品質改良米ぬかワックス
JP4936273B2 (ja) * 2005-03-01 2012-05-23 ボーソー油脂株式会社 精製ライスワックスの製造方法
JP5895248B2 (ja) * 2011-11-17 2016-03-30 株式会社トキワ 油性固形化粧料

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019097535A1 (fr) * 2017-11-20 2019-05-23 Praj Industries Limited Purification de cires à haute pression
JP2021503535A (ja) * 2017-11-20 2021-02-12 プラジ インダストリーズ リミテッドＰｒａｊ Ｉｎｄｕｓｔｒｉｅｓ Ｌｉｍｉｔｅｄ ロウの高圧精製
US10954470B2 (en) 2017-11-20 2021-03-23 Praj Industries Limited High pressure purification of waxes
JP7053829B2 (ja) 2017-11-20 2022-04-12 プラジ インダストリーズ リミテッド ロウの高圧精製
CN110607204A (zh) * 2019-10-29 2019-12-24 江苏京晶光电科技有限公司 一种从蓝宝石贴片废料中对液态蜡回收方法

Also Published As

Publication number Publication date
PH12017501626A1 (en) 2018-02-12
WO2016142953A3 (fr) 2016-10-27
JP2018510940A (ja) 2018-04-19
JP7150434B2 (ja) 2022-10-11

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