CN106563387A - Method for preparing PEG (polyethylene glycol) aliphatic ester surfactant from rice bran oil with low acid value - Google Patents

Method for preparing PEG (polyethylene glycol) aliphatic ester surfactant from rice bran oil with low acid value Download PDF

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Publication number
CN106563387A
CN106563387A CN201610992655.0A CN201610992655A CN106563387A CN 106563387 A CN106563387 A CN 106563387A CN 201610992655 A CN201610992655 A CN 201610992655A CN 106563387 A CN106563387 A CN 106563387A
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China
Prior art keywords
rice bran
bran oil
oil
peg600
acid value
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CN201610992655.0A
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Chinese (zh)
Inventor
金荣珍
金永
王方甫
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Anhui Province Yingshang County Sanjin Grain And Oil Co Ltd
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Anhui Province Yingshang County Sanjin Grain And Oil Co Ltd
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Priority to CN201610992655.0A priority Critical patent/CN106563387A/en
Publication of CN106563387A publication Critical patent/CN106563387A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/32—Polymers modified by chemical after-treatment
    • C08G65/329—Polymers modified by chemical after-treatment with organic compounds
    • C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
    • C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
    • C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
    • 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
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • 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
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • 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
    • C11B3/10—Refining fats or fatty oils by adsorption
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Microbiology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Materials Engineering (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)

Abstract

The invention discloses a method for preparing a PEG (polyethylene glycol) aliphatic ester surfactant from rice bran oil with low acid value. The method is characterized by being prepared from rice bran, alkaline protease, activated clay, activated carbon and PEG600 as raw materials. Grease in the rice bran is extracted with an aqueous enzymatic method, an oil extraction technology based on the aqueous enzymatic method is safe, environment-friendly and green, and obtained vegetable oil is pollution-free; the activated clay and the activated carbon are added for decolorize the rice bran oil; a supercritical CO2 extraction technology has the advantages of being high in extraction rate, good in selectivity and free of solvent residues and adopting a simple process and the like, can simplify a rice bran oil refining process and increases a refining yield of the rice bran oil; the rice bran oil is subjected to deacidification with a molecular distillation technology, and the molecular distillation technology is a grease deacidification technology and has the advantage of low energy consumption, small damage to grease, cleanliness and the like.

Description

A kind of method that low-acid value rice bran oil prepares PEG fatty acid surfactants
Technical field
The present invention relates to the preparation method application of rice bran oil, and in particular to a kind of low-acid value rice bran oil prepares PEG fat The method of fatty acid ester surface active agent.
Background technology
China is eating rice production state maximum in the world, and rice bran is the important by-products in rice process, and rice bran In fat content it is high, be a kind of important oil sources.Rice bran oil has containing various as a kind of new type natural vegetable oil to health The sp act composition of benefit.Rice bran oil has enhance immunity, reduces cholesterol, adjust blood fat, prevent the functions such as artery sclerosis, It is of high nutritive value.Rice bran oil is increasingly subject to the attention and favor of consumer because of abundant nutritive value and health care.
Xie Ying is in its master thesis《Rice bran oil produce and refinery practice research》In with fresh rice bran as raw material, with Optimization rice bran microwave technique is target, chooses ten kinds of organic solvents and extracts rice bran oil, optimal by orthogonal experiment optimization Microwave technique, have studied degumming, dewaxing, decolouring, the depickling step in Rice bran crude oil refinery practice.Organic solvent is leached Legal system oil oil yield is high, but, the use of organic solvent has potential safety hazard, and refinery practice is excessively loaded down with trivial details.
With rice bran as raw material, using the grease in aqueous enzymatic extraction rice bran, aqueous enzymatic method carries oil tech safety, ring to the present invention Guarantor, green, the vegetable oil of acquisition is pollution-free；Atlapulgite and activated carbon are added, desolventing technology is carried out to rice bran oil；Overcritical extraction The technology of taking has the advantages that high recovery rate, selective good, process is simple, no solvent residue, can simplify next step refining of crude rice bran oil Technological process, improves the refining yield of rice bran oil；The present invention carries out depickling process to rice bran oil using molecular distillation technique, and molecule steams The technology of evaporating is a kind of lipin deacidifying technology, has the advantages that energy consumption is low, little, cleaning is destroyed to grease.
The content of the invention
The invention mainly solves the technical problem of providing a kind of low-acid value rice bran oil prepares PEG fatty acid ester surface-actives The method of agent, the rice bran oil acid number prepared according to the technique is low, quality better.
The technical problem to be solved is realized using following technical scheme：
Rice bran 40-57, alkali protease 5-12, atlapulgite 4-10, activated carbon 3-9, PEG600 5-10, the concentrated sulfuric acid, distilled water In right amount.
A kind of method that low-acid value rice bran oil prepares PEG fatty acid surfactants, it is characterised in that according to the following steps Carry out：
A. rice bran is crossed into 40-60 mesh sieves, the regulation moisture content that adds water is 20-30%, is loaded in heat-resisting plate, is paved into 1-6cm thick simultaneously Stand is even, in being placed in micro-wave oven, takes out after 700-1000W, heating 90-180s, is cooled to room temperature, standby；
B. resulting material in a is placed in into supercritical CO2In extraction equipment, in 40-60 DEG C, CO2Flow 45-60kg/h, pressure Under 35-50MPa, 1-2h is extracted；
C. gained rice bran in b is added into alkali protease and water 1 through steam treatment:The mixture of 7-9, tune pH is 8-10, In 50-60 DEG C of stirring enzymolysis 4-6h, centrifugation obtains free oil A and emulsion；Emulsion is heated to into 90-100 DEG C, is stirred continuously Boiling 20-40min, is centrifuged obtaining free oil B, and both are mixed to get rice bran oil；
D. resulting material in c is heated to into 110-150 DEG C, adds atlapulgite and activated carbon, be stirred continuously, decolouring 1-2h takes out Filter；
E. resulting material in d is added in molecular clock instrument, opens cooling water, fill it up with liquid nitrogen, vacuumize, rice bran oil is carried out Preheating, stirring, in molecular clock rotating speed 180-240r/min, charging rate 2-5mL/min, pressure 1.0 × 10-7MPa, molecule steam Under the conditions of evaporating temperature 150-210 DEG C, 2-4h is processed, obtain a kind of rice bran oil of low acid number-high-quality；
F. by gained rice bran oil in e and PEG600 mixing, stir, be warming up to 100-120 DEG C, be slowly added to the concentrated sulfuric acid, instead 3-5h is answered, room temperature is cooled to, PEG600 fatty acid surfactants are obtained.
The reaction mechanism of the present invention is as follows：
（1）Supercritical extraction technique has the advantages that high recovery rate, selective good, process is simple, no solvent residue, under can simplifying One step refining of crude rice bran oil technological process, improves the refining yield of rice bran oil.
（2）With rice bran as raw material, using the grease in aqueous enzymatic extraction rice bran, it is safe and environment-friendly, green that aqueous enzymatic method carries oil tech Color, the vegetable oil of acquisition is pollution-free.
（3）Atlapulgite and activated carbon are added, desolventing technology is carried out to rice bran oil.
（4）The present invention carries out depickling process to rice bran oil using molecular distillation technique, and molecular distillation technique is a kind of grease Deacidification technique, has the advantages that energy consumption is low, little, cleaning is destroyed to grease.
（5）With the free fatty and PEG600 in rice bran oil as reaction raw materials, with the concentrated sulfuric acid as catalyst, prepare PEG600 fatty acid ester green surfactants.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of method that low-acid value rice bran oil prepares PEG fatty acid surfactants, by the raw material of following weight parts (g) It is obtained：
Rice bran 57, alkali protease 12, atlapulgite 10, activated carbon 9, PEG600 10, the concentrated sulfuric acid, distillation appropriate amount of water.
A kind of method that low-acid value rice bran oil prepares PEG fatty acid surfactants, it is characterised in that according to the following steps Carry out：
A. rice bran is crossed into 50 mesh sieves, the regulation moisture content that adds water is 20%, is loaded in heat-resisting plate, is paved into 5cm thickness and spreads out even, be placed in In micro-wave oven, take out after 800-900W, heating 180s, be cooled to room temperature, it is standby；
B. resulting material in a is placed in into supercritical CO2In extraction equipment, in 50-60 DEG C, CO2Flow 50-60kg/h, pressure Under 40-50MPa, 2h is extracted；
C. gained rice bran in b is added into alkali protease and water 1 through steam treatment:8 mixture, tune pH is 8-9, in 50-60 DEG C of stirring enzymolysis 4h, centrifugation obtains free oil A and emulsion；Emulsion is heated to into 90-100 DEG C, boiling is stirred continuously 40min, is centrifuged obtaining free oil B, and both are mixed to get rice bran oil；
D. resulting material in c is heated to into 120-130 DEG C, adds atlapulgite and activated carbon, be stirred continuously, decolouring 1h takes out Filter；
E. resulting material in d is added in molecular clock instrument, opens cooling water, fill it up with liquid nitrogen, vacuumize, rice bran oil is carried out Preheating, stirring, in molecular clock rotating speed 200-220r/min, charging rate 4-5mL/min, pressure 1.0 × 10-7MPa, molecule steam Under the conditions of evaporating temperature 180-200 DEG C, 2h is processed, obtain a kind of rice bran oil of low acid number-high-quality；
F. by gained rice bran oil in e and PEG600 mixing, stir, be warming up to 110-120 DEG C, be slowly added to the concentrated sulfuric acid, instead 4h is answered, room temperature is cooled to, PEG600 fatty acid surfactants are obtained.
Low acid number-high-quality rice bran oil performance test results prepared by above-described embodiment are as follows：
Acid number is 1.05mg KOH/g, and acid number reaches rice bran oil country three-level oil standard；
Peroxide value is 2.51mmol/kg, and peroxide value reaches the country-level oil standard of rice bran oil；
Oryzanol content is 3.16%, reaches rice bran oil national grade ii standard.

Claims (2)

1. a kind of method that low-acid value rice bran oil prepares PEG fatty acid surfactants, it is characterised in that by following weight parts Raw material be obtained：
Rice bran 40-57, alkali protease 5-12, atlapulgite 4-10, activated carbon 3-9, PEG600 5-10, the concentrated sulfuric acid, distilled water In right amount.
2. the method that a kind of low-acid value rice bran oil according to claim 1 prepares PEG fatty acid surfactants, it is special Levy and be, carry out according to the following steps：
A. rice bran is crossed into 40-60 mesh sieves, the regulation moisture content that adds water is 20-30%, is loaded in heat-resisting plate, is paved into 1-6cm thick simultaneously Stand is even, in being placed in micro-wave oven, takes out after 700-1000W, heating 90-180s, is cooled to room temperature, standby；
B. resulting material in a is placed in into supercritical CO2In extraction equipment, in 40-60 DEG C, CO2Flow 45-60kg/h, pressure 35- Under 50MPa, 1-2h is extracted；
C. gained rice bran in b is added into alkali protease and water 1 through steam treatment:The mixture of 7-9, tune pH is 8-10, In 50-60 DEG C of stirring enzymolysis 4-6h, centrifugation obtains free oil A and emulsion；Emulsion is heated to into 90-100 DEG C, is stirred continuously Boiling 20-40min, is centrifuged obtaining free oil B, and both are mixed to get rice bran oil；
D. resulting material in c is heated to into 110-150 DEG C, adds atlapulgite and activated carbon, be stirred continuously, decolouring 1-2h takes out Filter；
E. resulting material in d is added in molecular clock instrument, opens cooling water, fill it up with liquid nitrogen, vacuumize, rice bran oil is carried out Preheating, stirring, in molecular clock rotating speed 180-240r/min, charging rate 2-5mL/min, pressure 1.0 × 10-7MPa, molecule steam Under the conditions of evaporating temperature 150-210 DEG C, 2-4h is processed, obtain a kind of rice bran oil of low acid number-high-quality；
F. by gained rice bran oil in e and PEG600 mixing, stir, be warming up to 100-120 DEG C, be slowly added to the concentrated sulfuric acid, instead 3-5h is answered, room temperature is cooled to, PEG600 fatty acid surfactants are obtained.
CN201610992655.0A 2016-11-11 2016-11-11 Method for preparing PEG (polyethylene glycol) aliphatic ester surfactant from rice bran oil with low acid value Pending CN106563387A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108049224A (en) * 2017-12-07 2018-05-18 珠海宏河纺织材料有限公司 A kind of preparation method of the highly concentrated polyester modification surfactant of bipseudoindoxyl dye

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226126A (en) * 2011-04-27 2011-10-26 王金玲 Simplified preparation technology of rice oil
CN102295986A (en) * 2011-08-03 2011-12-28 中南林业科技大学 Preparation method of rice bran oil with low acid value
CN103409241A (en) * 2013-08-09 2013-11-27 丽江先锋食品开发有限公司 Preparation method of herbal elsholtzia essential oil
CN105062671A (en) * 2015-08-31 2015-11-18 江西省硒海油脂有限公司 Technology for refining rice bran oil from rice bran

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226126A (en) * 2011-04-27 2011-10-26 王金玲 Simplified preparation technology of rice oil
CN102295986A (en) * 2011-08-03 2011-12-28 中南林业科技大学 Preparation method of rice bran oil with low acid value
CN103409241A (en) * 2013-08-09 2013-11-27 丽江先锋食品开发有限公司 Preparation method of herbal elsholtzia essential oil
CN105062671A (en) * 2015-08-31 2015-11-18 江西省硒海油脂有限公司 Technology for refining rice bran oil from rice bran

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
宋小平等: "《精细化工品实用生产技术手册 表面活性剂 处理剂及润滑油制造技术》", 30 September 2006, 科学技术文献出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108049224A (en) * 2017-12-07 2018-05-18 珠海宏河纺织材料有限公司 A kind of preparation method of the highly concentrated polyester modification surfactant of bipseudoindoxyl dye

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