CN106978259A

CN106978259A - A kind of supercritical CO2The method of hydrogenated rice bran wax under system

Info

Publication number: CN106978259A
Application number: CN201710282552.XA
Authority: CN
Inventors: 潘明喆; 于殿宇; 齐晓芬; 李婷婷; 刘芳; 王立琦; 江连洲
Original assignee: Northeast Agricultural University
Current assignee: Northeast Agricultural University
Priority date: 2017-04-26
Filing date: 2017-04-26
Publication date: 2017-07-25

Abstract

The invention discloses a kind of supercritical CO₂The method of hydrogenated rice bran wax under system, it is characterized in that：In supercritical CO₂Under system, hydrogenation treatment is carried out to the rice bran wax after degumming using Pd/C as catalyst, the optimum response parameter of rice bran wax hydrogenation is obtained, after neutral oil in rice bran wax is hydrogenated, its oxidation stability and plasticity are improved, and the hydrogenated rear colour developing unit structure of partial pigment changes, and product colour is shoaled；The preparation time of the more conventional refined rice bran wax of the rice bran wax product on this condition shortens, and the problems such as efficiently solve dissolvent residual and cumbersome refining step, product iodine number is 55I₂G/100g, color is white, and physicochemical property is suitable with refined rice bran wax, can replace the refined application of rice bran wax in the industry.

Description

A kind of supercritical CO2The method of hydrogenated rice bran wax under system

Technical field

The present invention relates to a kind of supercritical CO₂The method of hydrogenated rice bran wax under system.

Background technology

China is world's production meter great Guo, and yield accounts for more than 1/3rd of Gross World Product.Rice bran is Rice producing Byproduct, general rice contains chaff 5%~8%, and fresh rice bran oil-containing is 16%~22% (W/W).Rice bran wax is rice bran oil refining The accessory substance of process, the ester mixture being made up of higher fatty acids and high alcohol, with synthetic wax and animal wax phase Than having the advantages that nontoxic.The wax paste produced during early stage production rice bran oil is all taken as waste disposal, with grinding in recent years That studies carefully deepens continuously, and has engendered the factory of processing rice bran wax, but there is technology mostly immature, small scale, equipment Simple and crude the problem of, the rice bran wax product generally existing of production is of poor quality, and oil-containing is high, the problems such as color and luster is deep, and general oil-containing is about 36.18%~84.71%, therefore the direct industrial use of wax paste is little, and industrially have through refined chaff wax and widely should With value, rice bran wax possesses very big potentiality in cosmetics, pharmacy, food, polymer, leather industry.

Due to contain colloid, the impurity such as neutral oil and pigment, therefore rice bran wax in brown shorts wax it is refined be generally divided into it is de- Glue, de-oiling, three steps of decolourizing.Subtractive process is cumbersome, and has used substantial amounts of chemical reagent, is unfavorable for environment and product Quality safety, and processing charges is higher.Asked to reduce chemical agent residue and expense height etc. in refining step, subtractive process Topic, using supercritical CO₂Under the conditions of degumming rice bran wax is hydrogenated, in addition to solving the above problems, the neutrality in rice bran wax After oil is hydrogenated, its oxidation stability and plasticity are improved, and the hydrogenated rear colour developing unit structure of partial pigment changes, and makes Product colour shoals.Obtained product has identical property with refined rice bran wax, in addition CO₂Be a kind of nontoxic, inertia, into Sheet is low, can be recycled, to the reaction medium of environment quite close friend.At present, traditional rice bran wax process for refining is gradually ripe, Through achieving preferable progress, but still need to new breakthrough.Therefore, the present invention proposes a kind of new rice bran wax processing method, obtains Go out in supercritical CO₂The optimal processing parameter of hydrogenated rice bran wax under system, improves the quality of rice bran wax, makes it industrially Have broad prospects.

The content of the invention

The present invention is in supercritical CO₂Under system, the rice bran wax after degumming is hydrogenated using Pd/C as catalyst Processing, has obtained the optimum response parameter of rice bran wax hydrogenation, on this condition, the hydrogenation time is shorter, product colour Shallow, physicochemical property is preferable, and preparation technology is simple, pollution-free, can replace the refined rice bran wax in some products.

Embodiment：

Embodiment one：

Step one：50g rice bran wax and the DG- adsorbents of rice bran wax quality 10% are weighed in container, and is put into stirring It is centrifuged after 85 DEG C, constant temperature stirring 75min are increased in heater, obtains degumming rice bran wax；

Step 2：100g degumming rice bran wax and 1,2,3,4,5% Pd/C catalyst into 150mL stainless steel kettles, plus Enter after rotor and to seal reactor, 2~6MPa CO is then injected into stainless steel cauldron₂Gas, carries out leak test, then use CO₂ Air in displacement stainless steel cauldron 3~5 times, its pressure is less than 5MPa；Then H is filled with into stainless steel cauldron₂Gas, Pressure be 5,6,7,8,9MPa, be re-filled with CO₂Total gas pressure is 14MPa；Put it into magnetic agitation oil bath pan, regulation turns Speed is 200,250,300,350,400r/min, temperature is 100,110,120,130,140 DEG C, the reaction time is 60,80,100, 120、140min；After reaction, the iodine number and color and luster of the reaction product are surveyed.

Embodiment two：Present implementation is that Pd/C is chosen in step 2 to be urged with the difference of specific implementation method one Agent consumption is 2,3,4%, and other compositions and step are identical with embodiment one.

Embodiment three：Present implementation is in step 2 to choose reactor with the difference of specific implementation method one Middle H₂Pressure be 6,7,8MPa, other compositions and step are identical with embodiment one.

Embodiment four：Present implementation is that rotating speed is chosen in step 2 is with the difference of specific implementation method one 250th, 300,350r/min, other compositions and step are identical with embodiment one.

Embodiment five：Present implementation is in step 2 to choose oil bath temperature with the difference of specific implementation method one Spend for 110,120,130 DEG C, other compositions and step are identical with embodiment one.

Embodiment six：When present implementation is to choose reaction in step 2 with the difference of specific implementation method one Between for 80,100,120min, other compositions and step are identical with embodiment one.

Claims

1. a kind of supercritical CO₂The method of hydrogenated rice bran wax under system, it is characterised in that following steps：

Step one：50g rice bran wax and the DG- adsorbents of rice bran wax quality 10% are weighed in container, and is put into agitating and heating It is centrifuged after 85 DEG C, constant temperature stirring 75min are increased in device, obtains degumming rice bran wax；

Step 2：100g degumming rice bran wax and 1,2,3,4,5% Pd/C catalyst into 150mL stainless steel kettles, add and turn Reactor is sealed after son, 2~6MPa CO is then injected into stainless steel cauldron₂Gas, carries out leak test, then use CO₂Displacement Air in stainless steel cauldron 3~5 times, its pressure is less than 5MPa；Then H is filled with into stainless steel cauldron₂Gas, pressure For 5,6,7,8,9MPa, be re-filled with CO₂Total gas pressure is 14MPa；Put it into magnetic agitation oil bath pan, regulation rotating speed is 200th, 250,300,350,400r/min, temperature is 100,110,120,130,140 DEG C, the reaction time is 60,80,100,120, 140min；After reaction, the iodine number and color and luster of the reaction product are surveyed.

2. a kind of supercritical CO according to claim 1₂The method of hydrogenated rice bran wax under system, it is characterised in that step 2 Middle selection Pd/C catalyst amounts are 2,3,4%.

3. a kind of supercritical CO according to claim 1₂The method of hydrogenated rice bran wax under system, it is characterised in that step 2 H in middle selection reactor₂Pressure be 6,7,8MPa.

4. a kind of supercritical CO according to claim 1₂The method of hydrogenated rice bran wax under system, it is characterised in that step 2 It is middle selection rotating speed be 250,300,350r/min.

5. a kind of supercritical CO according to claim 1₂The method of hydrogenated rice bran wax under system, it is characterised in that step 2 Middle selection oil bath temperature is 110,120,130 DEG C.

6. a kind of supercritical CO according to claim 1₂The method of hydrogenated rice bran wax under system, it is characterised in that step 2 It is middle selection the reaction time be 80,100,120min.