阅读说明：本技术 一种利用活性炭精制四级稻米油的方法及其产品 (Method for refining four-grade rice oil by using active carbon and product thereof ) 是由 王傲 蒋剑春 孙康 徐茹婷 孙昊 许伟 刘艳艳 陈超 卢辛成 于 2019-09-30 设计创作，主要内容包括：本发明公开了一种利用活性炭精制四级稻米油的方法及其产品,属于油脂精制技术领域。该方法利用糖脱色活性炭吸附四级稻米油中的顽固色素,25-100℃下震荡15-120min,真空过滤分离,得到一级稻米油；再利用溶剂法将糖脱色活性炭再生。该方法反应条件温和,能耗低,精制过程不产生毒副产物；所使用的糖脱色活性炭使用后可再生,再生溶剂也可回收,不产生废水、废气及固废污染；通过活性炭再生溶剂的筛选可实现谷维素和叶红素的分别富集分离。再生分离得到的谷维素可返填至一级稻米油中实现稻米油中谷维素无损,也可作为药物、食品添加剂等使用。本发明可为四级稻米油的精制以及谷维素等营养成分的分离提纯提供了参考和借鉴。(The invention discloses a method for refining four-grade rice oil by using activated carbon and a product thereof, belonging to the technical field of oil refining. Adsorbing stubborn pigments in the four-grade rice oil by using sugar decolorizing active carbon, shaking for 15-120min at 25-100 ℃, and performing vacuum filtration and separation to obtain first-grade rice oil; and regenerating sugar decolorizing active carbon by a solvent method. The method has mild reaction conditions, low energy consumption and no toxic by-products generated in the refining process; the used sugar decolorizing active carbon can be regenerated after use, and the regenerated solvent can also be recovered, so that the pollution of waste water, waste gas and solid waste is not generated; the respective enrichment and separation of oryzanol and phytoene can be realized by screening the activated carbon regeneration solvent. The oryzanol obtained by regeneration and separation can be filled back into first-grade rice oil to realize no loss of oryzanol in the rice oil, and can also be used as medicine, food additive, etc. The invention can provide reference for the refining of the four-grade rice oil and the separation and purification of nutrient components such as oryzanol and the like.)

1. A method for refining four-grade rice oil by using activated carbon is characterized in that sugar decolorizing activated carbon is added into the four-grade rice oil, the four-grade rice oil is shaken for 15-120min at 25-100 ℃, and vacuum filtration and separation are carried out to obtain the first-grade rice oil.

2. The method for refining rice quaternary oil by using activated carbon as claimed in claim 1, wherein the mass ratio of the rice quaternary oil to the sugar decolorizing activated carbon is 1: 0.05-0.3.

3. The method for refining rice quaternary oil with activated carbon as claimed in claim 1, wherein the mass ratio of rice quaternary oil to sugar decolorizing activated carbon is 1: 0.1.

4. The method for refining rice quaternary oil with activated carbon as claimed in claim 1, wherein sugar decolorizing activated carbon is added to rice quaternary oil and shaken at 50 ℃ for 30 min.

5. The method for refining rice quaternary oil by using activated carbon according to claim 1, wherein the sugar decolorizing activated carbon has an A-caramel decolorization ratio of 110 to 130%.

6. The method for refining rice quaternary oil by using activated carbon according to claim 1, wherein sugar decolorizing activated carbon obtained by vacuum filtration separation is regenerated by a solvent method, comprising the steps of:

(1) at normal temperature, adding an organic solvent A into sugar decolorizing active carbon collected after reaction, washing and filtering, repeating for 3 times, marking the obtained active carbon as RAC1, evaporating the washed filtrate to remove the solvent, recycling the solvent, and marking the residue as O1; the organic solvent A is one or a mixture of more of n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil;

(2) adding an organic solvent B into the RAC1 obtained in the step (1), washing and filtering, repeating for 3 times, recording the activated carbon as RAC2, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O2; the organic solvent B is one or a mixture of more of ethyl acetate, chloroform, dichloromethane, n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil;

(3) adding an organic solvent C into the RAC2 obtained in the step (2), washing and filtering, repeating for 3 times, recording the activated carbon as RAC3, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O3; the organic solvent C is one or a mixture of more of chloroform, dichloromethane, ethyl acetate, n-hexane, cyclohexane, n-heptane, petroleum ether or solvent oil VI.

7. The method for refining rice quaternary oil with activated carbon according to claim 1, wherein the volume-to-mass ratio of the addition amount of each organic solvent to the sugar decolorizing activated carbon in the organic solvent A, the organic solvent B and the organic solvent C is 5-10 mL: 1 g.

8. A method for refining rice quaternary oil with activated carbon according to claim 1, comprising the steps of:

(1) adding sugar decolorizing active carbon into four-grade rice oil, shaking at 25-100 deg.C for 15-120min, vacuum filtering and separating to obtain first-grade rice oil; then, carrying out solvent method regeneration on the sugar decolorizing active carbon;

(2) at normal temperature, adding an organic solvent A into sugar decolorizing active carbon collected after reaction, washing and filtering, repeating for 3 times, marking the obtained active carbon as RAC1, evaporating the washed filtrate to remove the solvent, recycling the solvent, and marking the residue as O1; the organic solvent A is one or a mixture of more of n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil; the volume-mass ratio of the addition amount of the organic solvent A to the sugar decolorizing active carbon is 5-10 mL: 1 g;

(3) adding an organic solvent B into the RAC1 obtained in the step (2), washing and filtering, repeating for 3 times, recording the activated carbon as RAC2, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O2; the organic solvent B is one or a mixture of more of ethyl acetate, chloroform, dichloromethane, n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil; the volume-mass ratio of the addition amount of the organic solvent B to the sugar decolorizing active carbon is 5-10 mL: 1 g;

(4) adding an organic solvent C into the RAC2 obtained in the step (3), washing and filtering, repeating for 3 times, recording the activated carbon as RAC3, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O3; the organic solvent C is one or a mixture of more of chloroform, dichloromethane, ethyl acetate, n-hexane, cyclohexane, n-heptane, petroleum ether or solvent oil VI; the volume-mass ratio of the addition amount of the organic solvent C to the sugar decolorizing active carbon is 5-10 mL: 1 g;

(5) the activated carbon RAC3 was used continuously for the next round of refining of the fourth grade rice oil.

9. The method for refining rice quaternary oil by using activated carbon as claimed in claim 1, wherein O2 is added to the prepared rice primary oil, and the mass ratio of the added O2 to the rice primary oil is 0.025-0.05: 1.

10. A first grade rice oil prepared by the method for refining a fourth grade rice oil by using activated carbon according to any one of claims 1 to 9.

Technical Field

The invention belongs to the technical field of oil refining, and particularly relates to a method for refining rice oil by using activated carbon and a product thereof.

Background

Rice oil, also known as rice bran oil, is a natural oil extracted from rice bran, a byproduct of rice processing. The rice oil is rich in multiple physiologically active substances such as oryzanol, phytosterol, vitamin E, squalene shark and the like, and the ratio of linoleic acid to oleic acid is 1: 1.1, which meets the optimal ratio recommended by the world health organization. The long-term consumption of rice oil has the effects of reducing cholesterol content in blood, lowering blood pressure, regulating autonomic nerve, and preventing cardiovascular and cerebrovascular diseases. In view of this, rice bran oil (rice oil) was listed as the best edible oil together with corn oil and sesame oil at the 113 th conference of the world health organization in 2010.

After crude oil is extracted from rice bran, the crude oil is generally refined by degumming, deacidification, decoloration, deodorization, dewaxing and other processes. The stubborn pigments in the rice oil are difficult to remove by the conventional process, so the obtained rice oil is generally red brown, can only reach the four-grade rice oil standard specified in GB/T22460, and seriously affects the quality and the sale price of the rice oil.

Conventional four-stage rice oil refining methods include a chemical alkali refining method, a molecular distillation method, a physical adsorption method, and the like. The chemical alkali refining method comprises the steps of adding sodium hydroxide into rice oil for alkali refining, extracting the oryzanol by using a sodium hydroxide solution of methanol, and adsorbing and removing the pigment in the rice oil by using an adsorbent. The method has complicated steps, needs strong alkali in the refining process, generates solid waste, is easy to cause environmental pollution, and also can cause great loss of nutrient components in the rice oil. The invention patents ZL201410016377.6 and ZL201410016379.5 describe refining of four-grade rice oil by molecular distillation. The molecular distillation belongs to a physical method, no chemical reagent is used in the process, no wastewater pollution is generated, and the nutrient components in the rice oil can be retained to the maximum extent. However, molecular distillation generally requires high vacuum and high temperature, energy consumption is large, process conditions are harsh, and the high-temperature distillation process may also cause generation and enrichment of toxic substances such as chloropropanol ester and the like, so that the quality of refined rice oil is affected, and potential safety hazards are generated. The conventional adsorbing material has the defects of high price, weak selective adsorption, non-regeneration, solid waste generation, even dangerous waste generation and large loss of rice oil and nutrient substances.

Disclosure of Invention

The invention solves the technical problems that the refining of the four-grade rice oil in the prior art generally needs high vacuum and high temperature, has large energy consumption and harsh process conditions, and can also cause the generation and enrichment of toxic substances such as chloropropanol ester and the like, thereby influencing the quality of the refined rice oil and generating potential safety hazard. The conventional adsorbing material has the defects of high price, weak selective adsorption, non-regeneration, solid waste generation, even dangerous waste generation and large loss of rice oil and nutrient substances.

In order to solve the problems, the technical scheme adopted by the invention is as follows:

a method for refining four-grade rice oil with activated carbon comprises adding sugar decolorizing activated carbon into four-grade rice oil, shaking at 25-100 deg.C for 15-120min, and vacuum filtering for separation to obtain first-grade rice oil.

According to the method for refining the four-grade rice oil by using the activated carbon, the mass ratio of the four-grade rice oil to the sugar decolorizing activated carbon is 1: 0.05-0.3.

According to the method for refining the four-grade rice oil by using the activated carbon, the mass ratio of the four-grade rice oil to the sugar decolorizing activated carbon is 1: 0.1.

The method for refining the four-grade rice oil by using the activated carbon comprises the steps of adding sugar decolorizing activated carbon into the four-grade rice oil, and shaking for 30min at 50 ℃.

According to the method for refining the four-grade rice oil by using the activated carbon, the A-caramel decolorization rate of the sugar decolorization activated carbon is 110-130%.

The method for refining the four-grade rice oil by using the activated carbon is characterized in that sugar decoloration activated carbon obtained by vacuum filtration and separation is regenerated by a solvent method, and comprises the following steps:

(1) at normal temperature, adding an organic solvent A into sugar decolorizing active carbon collected after reaction, washing and filtering, repeating for 3 times, marking the obtained active carbon as RAC1, evaporating the washed filtrate to remove the solvent, recycling the solvent, and marking the residue as O1; the organic solvent A is one or a mixture of more of n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil, and is mainly used for separating and recovering rice oil in the adsorption saturated activated carbon;

(2) adding an organic solvent B into the RAC1 obtained in the step (1), washing and filtering, repeating for 3 times, recording the activated carbon as RAC2, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O2; the organic solvent B is one or a mixture of more of ethyl acetate, chloroform, dichloromethane, n-hexane, cyclohexane, n-heptane, petroleum ether or number six solvent oil, and is mainly used for enriching and recovering nutrient substances in the adsorption saturated activated carbon;

(3) adding an organic solvent C into the RAC2 obtained in the step (2), washing and filtering, repeating for 3 times, recording the activated carbon as RAC3, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O3; the organic solvent C is one or a mixture of more of chloroform, dichloromethane, ethyl acetate, n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil, and is mainly used for enriching and recovering pigments in the adsorption saturated activated carbon.

According to the method for refining the four-grade rice oil by using the activated carbon, the volume-mass ratio of the addition amount of each organic solvent to the activated carbon in the organic solvent A, the organic solvent B and the organic solvent C is 5-10 mL: 1 g.

The method for refining the four-grade rice oil by using the activated carbon is characterized by comprising the following steps of:

(1) adding sugar decolorizing active carbon into four-grade rice oil, shaking at 25-100 deg.C for 15-120min, vacuum filtering and separating to obtain first-grade rice oil; then, carrying out solvent method regeneration on the sugar decolorizing active carbon;

(2) at normal temperature, adding an organic solvent A into sugar decolorizing active carbon collected after reaction, washing and filtering, repeating for 3 times, marking the obtained active carbon as RAC1, evaporating the washed filtrate to remove the solvent, recycling the solvent, and marking the residue as O1; the organic solvent A is one or a mixture of more of n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil; the volume-mass ratio of the addition amount of the organic solvent A to the sugar decolorizing active carbon is 5-10 mL: 1 g;

(3) adding an organic solvent B into the RAC1 obtained in the step (2), washing and filtering, repeating for 3 times, recording the activated carbon as RAC2, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O2; the organic solvent B is one or a mixture of more of ethyl acetate, chloroform, dichloromethane, n-hexane, cyclohexane, n-heptane, petroleum ether or No. six solvent oil; the volume-mass ratio of the addition amount of the organic solvent B to the sugar decolorizing active carbon is 5-10 mL: 1 g;

(4) adding an organic solvent C into the RAC2 obtained in the step (3), washing and filtering, repeating for 3 times, recording the activated carbon as RAC3, evaporating the washed filtrate to remove the solvent, recycling the solvent, and recording the residue as O3; the organic solvent C is one or a mixture of more of chloroform, dichloromethane, ethyl acetate, n-hexane, cyclohexane, n-heptane, petroleum ether or solvent oil VI; the volume-mass ratio of the addition amount of the organic solvent C to the sugar decolorizing active carbon is 5-10 mL: 1 g;

(5) the activated carbon RAC3 was used continuously in the next round of refining of the fourth grade rice oil.

According to the method for refining the four-grade rice oil by using the activated carbon, O2 can be added into the prepared first-grade rice oil, and the mass ratio of the addition amount of O2 to the first-grade rice oil is 0.025-0.05: 1.

The first-grade rice oil is prepared by the method for refining the fourth-grade rice oil by using the active carbon.

Has the advantages that: compared with the prior art, the invention has the advantages that:

(1) the method has mild reaction conditions, does not need chemical reagents such as high temperature, high vacuum, strong alkali and the like, has low energy consumption, and does not generate toxic by-products in the refining process.

(2) The active carbon used in the refining process of the active carbon rice oil can be regenerated after being used, the regenerated solvent can also be recovered, the pollution of waste water, waste gas and solid waste is not generated, and the comprehensive cost is greatly reduced.

(3) The invention can realize the respective enrichment and separation of nutrient substances (mainly oryzanol) and pigments (mainly lutein) by screening the activated carbon regeneration solvent; the obtained nutrient substances can be added into refined rice oil to realize no damage to the nutrient substances in the rice oil, and can also be used as medicine and food additive.

(4) The process of the invention provides reference for refining the active carbon rice oil and separating and purifying nutrient components such as oryzanol and the like.

Detailed Description

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.