CN113621441A - Preparation method of modified rice bran wax - Google Patents
Preparation method of modified rice bran wax Download PDFInfo
- Publication number
- CN113621441A CN113621441A CN202110895872.9A CN202110895872A CN113621441A CN 113621441 A CN113621441 A CN 113621441A CN 202110895872 A CN202110895872 A CN 202110895872A CN 113621441 A CN113621441 A CN 113621441A
- Authority
- CN
- China
- Prior art keywords
- wax
- rice bran
- melting
- bran wax
- synthetic wax
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C5/00—Candles
- C11C5/002—Ingredients
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
- C09G1/08—Other polishing compositions based on wax
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to the technical field of rice bran wax, in particular to a preparation method of modified rice bran wax. The method is characterized by comprising the following steps: s1, adding concentrated sulfuric acid into the first enamel reaction kettle, adding rice bran wax, adding hydrogen peroxide solution under stirring, continuously stirring for 12-14 hours, and standing for 1 hour to separate wax and water; s2, remelting the oxidized rice bran wax in the upper layer into liquid, adding water while stirring, continuously stirring for 30-40 minutes, standing for 1-3 hours, and separating the wax and the water; s3, repeating the step S2 for 3-5 times; s4, mixing the high acid value synthetic wax with methyl isopropyl ketone, heating to a high acid value synthetic wax for complete dissolution, continuously and slowly stirring and cooling to a constant temperature of 45-55 ℃, and separating solid and liquid; s5, vacuum distilling the solid to obtain high melting point synthetic wax; and S6, carrying out vacuum distillation on the liquid to obtain the synthetic wax with low melting point. Compared with the prior art, the modified rice bran wax has the characteristics of natural wax and has the special properties of high brightness and easy emulsification.
Description
Technical Field
The invention relates to the technical field of rice bran wax, in particular to a preparation method of modified rice bran wax.
Background
The natural rice bran wax is mainly ester formed by higher fatty alcohol and higher fatty acid, has higher melting point and is precipitated at normal temperature, the rice bran wax is extracted from a byproduct wax paste refined from the rice bran oil, the quality of the rice bran oil is obviously improved, the extracted rice bran wax has due value in many aspects, and the rice bran wax is widely applied to the aspects of food, daily chemicals, chemical industry and the like.
However, the natural rice bran wax has single performance and cannot meet various requirements, and the natural rice bran wax needs to be modified. The Chinese patent with the application number of 201810001691.5 discloses rice bran wax acid ester wax and a preparation method thereof, wherein the rice bran wax acid ester wax after acid washing is directly subjected to esterification reaction, and the finally obtained rice bran wax acid ester wax has single performance and is not beneficial to re-synthesizing other synthetic waxes with various characteristics on the basis of the rice bran wax acid ester wax.
Therefore, the preparation method of the modified rice bran wax is designed, and the modified rice bran wax has the characteristics of natural wax and has the special properties of high brightness and easiness in emulsification.
Disclosure of Invention
The invention provides a preparation method of modified rice bran wax for overcoming the defects of the prior art, and the modified rice bran wax has the characteristics of natural wax and has the special properties of high brightness and easy emulsification.
In order to achieve the aim, the preparation method of the modified rice bran wax is characterized by comprising the following steps:
s1, adding concentrated sulfuric acid with the concentration of 75% into a first enamel reaction kettle, keeping the continuous heating state, adding rice bran wax into the first enamel reaction kettle, continuously heating the rice bran wax to 90-100 ℃ to melt the rice bran wax, slowly adding 35% hydrogen peroxide solution under the stirring state, continuously stirring for 12-14 hours under the constant temperature condition of 90-100 ℃ to completely oxidize the rice bran wax, naturally cooling the rice bran wax to light beige, standing for 1 hour to separate the wax from water, and discharging the water at the lower layer;
s2, heating the enamel reaction kettle to 90-100 ℃, re-melting the oxidized rice bran wax on the upper layer into liquid, adding water under stirring, continuously stirring for 30-40 minutes, standing for 1-3 hours, separating the wax and the water, and discharging the water on the lower layer;
s3, repeating the step S2 for 3-5 times, wherein the upper layer is the high-acid-value synthetic wax, and the lower layer is water recycled;
s4, mixing the high-acid-value synthetic wax with methyl isopropyl ketone, heating to a high-acid-value synthetic wax for complete dissolution, slowly cooling the mixed solution under continuous slow stirring to a constant temperature of 45-55 ℃, keeping the temperature for 30-40 minutes, and separating solid and liquid;
s5, vacuum distilling the solid to obtain high melting point synthetic wax;
s6, carrying out vacuum distillation on the liquid to obtain the synthetic wax with low melting point, wherein the distilled liquid is methyl isopropyl ketone and is reserved for subsequent recycling.
The mass ratio of the high-acid-value synthetic wax to the methyl isopropyl ketone in the step S4 is 1: 5.
And (3) putting the high-melting-point synthetic wax and zinc oxide into a second enamel reaction kettle, heating to 150-160 ℃ to melt the high-melting-point synthetic wax, adding ethylene glycol to react for 5-8 hours, and washing after the reaction is finished to obtain the first modified rice bran wax.
The mass ratio of the high-melting-point synthetic wax to the zinc oxide is 100:1, and the mass ratio of the high-melting-point synthetic wax to the ethylene glycol is 20: 1.
And (3) putting the high-melting-point synthetic wax and zinc oxide into a third enamel reaction kettle, heating to 150-160 ℃ to melt the high-melting-point synthetic wax, adding calcium oxide for reaction for 5-8 hours, and washing with water after the reaction is finished to obtain second modified rice bran wax.
The mass ratio of the high-melting-point synthetic wax to the zinc oxide is 100:1, and the mass ratio of the high-melting-point synthetic wax to the calcium oxide is 40: 1.
And (3) putting the low-melting-point synthetic wax and zinc oxide into a fourth enamel reaction kettle, heating to 150-160 ℃ to melt the low-melting-point synthetic wax, adding high-molecular polyethylene glycol, reacting for 5-8 hours, slowly cooling to normal temperature after the reaction is finished, and filtering to obtain a third modified rice bran wax emulsion.
The mass ratio of the low-melting-point synthetic wax to the zinc oxide is 100:1, and the mass ratio of the low-melting-point synthetic wax to the high-molecular polyethylene glycol is 100: 3.
And the third modified rice bran wax emulsion is subjected to a powder blowing process to obtain solid third modified rice bran wax.
The molecular weight of the high molecular polyethylene glycol is 400-600.
Compared with the prior art, the modified rice bran wax has the characteristics of natural wax and has the special properties of high brightness and easy emulsification.
Detailed Description
The first embodiment is as follows:
this example of a process for preparing a modified rice bran wax includes the steps of:
s1, adding 500kg of natural rice bran wax into a first enamel reaction kettle filled with 2200ml of concentrated sulfuric acid with concentration of 75% in a heating state, continuously heating to 90 ℃ to melt the rice bran wax, slowly adding 5000ml of hydrogen peroxide solution with concentration of 35% in a stirring state, continuously stirring for 12 hours at a constant temperature of 90 ℃ to completely oxidize the rice bran wax, wherein the color of the rice bran wax is changed into light beige, naturally cooling, standing for 1 hour to separate the wax from water, and discharging the lower water layer;
s2, heating the enamel reaction kettle to 90 ℃, re-melting the oxidized rice bran wax on the upper layer into liquid, adding water under stirring, continuously stirring for 30 minutes, standing for 1 hour, separating the wax and the water, and discharging the water on the lower layer;
s3, repeating the step S2 for 3-5 times, wherein the upper layer is the high-acid-value synthetic wax, and the lower layer is water recycled;
s4, mixing the high-acid-value synthetic wax with methyl isopropyl ketone, heating to a high-acid-value synthetic wax, completely dissolving, slowly cooling the mixed solution under continuous slow stirring to 45 ℃, keeping the temperature constant for 30 minutes, and separating solid and liquid, wherein the mass ratio of the high-acid-value synthetic wax to the methyl isopropyl ketone is 1: 5;
s5, vacuum distilling the solid to obtain high melting point synthetic wax;
s6, carrying out vacuum distillation on the liquid to obtain synthetic wax with a low melting point, wherein the distilled liquid is methyl isopropyl ketone and is reserved for subsequent recycling;
s7, putting 200kg of high-melting-point synthetic wax and 2kg of zinc oxide into a second enamel reaction kettle, heating to 150 ℃ to melt the high-melting-point synthetic wax, adding 10kg of ethylene glycol, reacting for 5-8 hours, and washing with water after the reaction is finished to obtain the first modified rice bran wax.
And (3) adding chromium oxide into the water washed out from the lower layer in the steps S2 and S3, and then adding glucose to perform a reduction reaction to prepare the leather tanning assisting kneading agent, wherein the washed water can be reused, and production resources are fully utilized.
The methyl isopropyl ketone in the step S4 is an easily obtained organic solvent, the boiling point of the methyl isopropyl ketone is 79.6 ℃, and the melting point of the methyl isopropyl ketone is matched with the melting point of the rice bran wax after acidification modification; the dissolving power is excellent, and the dissolving power is strong for the intermediate after the rice bran wax acidification modification; the intermediate before modification of the rice bran wax is dissolved in the methyl isopropyl ketone to be very stable, and the problems of decomposition, coking and the like can not be generated at high temperature; because the boiling point of the methyl isopropyl ketone is lower, the methyl isopropyl ketone is easier to remove in the vacuum distillation processes of the steps S5 and S6, the residue is less, and the influence on the synthetic wax is less.
In step S4, the high melting point synthetic wax precipitated in a solid state at 45 ℃ and the low melting point synthetic wax continued to exist in a solution state. After the wax is distinguished by melting points, high-melting point synthetic wax and low-melting point synthetic wax with different brightness and properties are obtained.
The high-melting-point synthetic wax has high brightness, and the brightness can be enhanced again through subsequent synthetic treatment on the basis to prepare the high-melting-point, high-hardness and high-brightness synthetic wax without causing uncontrollable or inconspicuous brightness improvement of a final product due to interference of the low-melting-point wax.
The self-emulsifying synthetic wax prepared by subsequent treatment of the low-melting-point synthetic wax has stable self-emulsifying performance and can not cause incomplete emulsification due to the existence of the high-melting-point wax with limited self-emulsifying performance.
In step S7, the high melting point synthetic wax and ethylene glycol undergo a dehydration esterification reaction under the catalytic action of zinc oxide, so as to obtain the first modified rice bran wax with high gloss, high hardness and easy emulsification.
Example two:
this example of a process for preparing a modified rice bran wax includes the steps of:
steps S1-S6 are the same as in the first embodiment;
and step S7, putting 200kg of high-melting-point synthetic wax and 2kg of zinc oxide into a third enamel reaction kettle, heating to 150 ℃ to melt the high-melting-point synthetic wax, adding 5kg of calcium oxide, reacting for 5-8 hours, and washing with water after the reaction is finished to obtain second modified rice bran wax.
In step S7, the high melting point synthetic wax undergoes saponification with calcium oxide under the catalytic action of zinc oxide to obtain a second modified rice bran wax with high hardness, good polishing performance, and high gloss.
Example three:
this example of a process for preparing a modified rice bran wax includes the steps of:
steps S1-S6 are the same as in the first embodiment;
step S7, putting 200kg of low-melting-point synthetic wax and 2kg of zinc oxide into a fourth enamel reaction kettle, heating to 150 ℃ to melt the low-melting-point synthetic wax, adding 6kg of high-molecular polyethylene glycol with the molecular weight of 400, reacting for 5-8 hours, slowly cooling to normal temperature after the reaction is finished, and filtering to obtain a third modified rice bran wax emulsion.
And step S8, performing a powder blowing process on the third modified rice bran wax emulsion to obtain solid third modified rice bran wax according to needs.
In step S7, the low melting point synthetic wax and the high molecular polyethylene glycol undergo a dehydration esterification reaction under the catalytic action of zinc oxide, so as to obtain a third modified rice bran wax emulsion with self-emulsifying property, and the third modified rice bran wax emulsion is soft and smooth in luster.
Claims (10)
1. A preparation method of modified rice bran wax is characterized by comprising the following steps:
s1, adding concentrated sulfuric acid with the concentration of 75% into a first enamel reaction kettle, keeping the continuous heating state, adding rice bran wax into the first enamel reaction kettle, continuously heating the rice bran wax to 90-100 ℃ to melt the rice bran wax, slowly adding 35% hydrogen peroxide solution under the stirring state, continuously stirring for 12-14 hours under the constant temperature condition of 90-100 ℃ to completely oxidize the rice bran wax, naturally cooling the rice bran wax to light beige, standing for 1 hour to separate the wax from water, and discharging the water at the lower layer;
s2, heating the enamel reaction kettle to 90-100 ℃, re-melting the oxidized rice bran wax on the upper layer into liquid, adding water under stirring, continuously stirring for 30-40 minutes, standing for 1-3 hours, separating the wax and the water, and discharging the water on the lower layer;
s3, repeating the step S2 for 3-5 times, wherein the upper layer is the high-acid-value synthetic wax, and the lower layer is water recycled;
s4, mixing the high-acid-value synthetic wax with methyl isopropyl ketone, heating to a high-acid-value synthetic wax for complete dissolution, slowly cooling the mixed solution under continuous slow stirring to a constant temperature of 45-55 ℃, keeping the temperature for 30-40 minutes, and separating solid and liquid;
s5, vacuum distilling the solid to obtain high melting point synthetic wax;
s6, carrying out vacuum distillation on the liquid to obtain the synthetic wax with low melting point, wherein the distilled liquid is methyl isopropyl ketone and is reserved for subsequent recycling.
2. The method of claim 1, further comprising the steps of: the mass ratio of the high-acid-value synthetic wax to the methyl isopropyl ketone in the step S4 is 1: 5.
3. The method of claim 1, further comprising the steps of: and (3) putting the high-melting-point synthetic wax and zinc oxide into a second enamel reaction kettle, heating to 150-160 ℃ to melt the high-melting-point synthetic wax, adding ethylene glycol to react for 5-8 hours, and washing after the reaction is finished to obtain the first modified rice bran wax.
4. The method of claim 3, wherein the modified rice bran wax is prepared by: the mass ratio of the high-melting-point synthetic wax to the zinc oxide is 100:1, and the mass ratio of the high-melting-point synthetic wax to the ethylene glycol is 20: 1.
5. The method of claim 1, further comprising the steps of: and (3) putting the high-melting-point synthetic wax and zinc oxide into a third enamel reaction kettle, heating to 150-160 ℃ to melt the high-melting-point synthetic wax, adding calcium oxide for reaction for 5-8 hours, and washing with water after the reaction is finished to obtain second modified rice bran wax.
6. The method of claim 5, wherein the modified rice bran wax is prepared by: the mass ratio of the high-melting-point synthetic wax to the zinc oxide is 100:1, and the mass ratio of the high-melting-point synthetic wax to the calcium oxide is 40: 1.
7. The method of claim 1, further comprising the steps of: and (3) putting the low-melting-point synthetic wax and zinc oxide into a fourth enamel reaction kettle, heating to 150-160 ℃ to melt the low-melting-point synthetic wax, adding high-molecular polyethylene glycol, reacting for 5-8 hours, slowly cooling to normal temperature after the reaction is finished, and filtering to obtain a third modified rice bran wax emulsion.
8. The method of claim 7, wherein the modified rice bran wax is prepared by: the mass ratio of the low-melting-point synthetic wax to the zinc oxide is 100:1, and the mass ratio of the low-melting-point synthetic wax to the high-molecular polyethylene glycol is 100: 3.
9. The method of claim 7, wherein the modified rice bran wax is prepared by: and the third modified rice bran wax emulsion is subjected to a powder blowing process to obtain solid third modified rice bran wax.
10. The method of claim 7, wherein the modified rice bran wax is prepared by: the molecular weight of the high molecular polyethylene glycol is 400-600.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110895872.9A CN113621441A (en) | 2021-08-05 | 2021-08-05 | Preparation method of modified rice bran wax |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110895872.9A CN113621441A (en) | 2021-08-05 | 2021-08-05 | Preparation method of modified rice bran wax |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113621441A true CN113621441A (en) | 2021-11-09 |
Family
ID=78382840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110895872.9A Withdrawn CN113621441A (en) | 2021-08-05 | 2021-08-05 | Preparation method of modified rice bran wax |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113621441A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897140A (en) * | 2021-11-15 | 2022-01-07 | 云南群英汽车服务有限公司 | Wax water oxidation process for automobile cleaning |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881753A (en) * | 2014-04-12 | 2014-06-25 | 曲靖众一精细化工股份有限公司 | Emulsion type wax refined by esterifying lignite wax and preparation method of emulsion type wax |
| CN108129302A (en) * | 2018-01-02 | 2018-06-08 | 重庆合才化工有限公司 | A kind of rice bran cerotate wax and preparation method thereof |
| CN108191602A (en) * | 2018-01-02 | 2018-06-22 | 重庆合才化工有限公司 | A kind of rice bran cerinic acid calcium soap wax and preparation method thereof |
| CN111004512A (en) * | 2019-12-25 | 2020-04-14 | 江门市德山复合材料科技有限公司 | Processing aid containing rice bran wax and preparation method thereof |
-
2021
- 2021-08-05 CN CN202110895872.9A patent/CN113621441A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881753A (en) * | 2014-04-12 | 2014-06-25 | 曲靖众一精细化工股份有限公司 | Emulsion type wax refined by esterifying lignite wax and preparation method of emulsion type wax |
| CN108129302A (en) * | 2018-01-02 | 2018-06-08 | 重庆合才化工有限公司 | A kind of rice bran cerotate wax and preparation method thereof |
| CN108191602A (en) * | 2018-01-02 | 2018-06-22 | 重庆合才化工有限公司 | A kind of rice bran cerinic acid calcium soap wax and preparation method thereof |
| CN111004512A (en) * | 2019-12-25 | 2020-04-14 | 江门市德山复合材料科技有限公司 | Processing aid containing rice bran wax and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897140A (en) * | 2021-11-15 | 2022-01-07 | 云南群英汽车服务有限公司 | Wax water oxidation process for automobile cleaning |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10465144B2 (en) | Method to recover free fatty acids from fats and oils | |
| US9353331B2 (en) | Method to recover free fatty acids from fats and oils | |
| US2240365A (en) | Method of treating tall oil | |
| CN113621441A (en) | Preparation method of modified rice bran wax | |
| CN101238889A (en) | Method for refining rice bran oil by mixing crude rice bran oil refining technique | |
| CN102061222A (en) | Method for continuously producing epoxidized soybean oil | |
| CN110818762A (en) | Residual oil treatment method for recovering sterol and refining sylvite | |
| CN110028542A (en) | The clean preparation method of canrenone | |
| Wafti et al. | Value-added products from palm sludge oil | |
| US2248346A (en) | Method for the recovery of phytosterol | |
| ITUA20164118A1 (en) | Preparation process of purified dicarboxylic acids. | |
| US2782216A (en) | Refining vegetable oils | |
| CN108373435A (en) | A kind of 1,1- is bis-（T-butylperoxy）The recoverying and utilizing method of -3,3,5- trimethyl-cyclohexane soda-wash waters | |
| CN113943606A (en) | Preparation method of wool essence and/or cashmere essence | |
| JP2003292987A (en) | Process for upgradation and bleaching of crude rice bran wax | |
| US3391191A (en) | Liquid phase decarboxylation of fatty acids to ketones | |
| US2640823A (en) | Treatment of tall oil | |
| CN105695105A (en) | Method for co-producing fatty acid methyl ester, vitamin E and phytosterol from carclazyte oil | |
| US2166812A (en) | Process for the separation of the constituents of organic mixtures containing both resin acids and fatty acids, particularly tall oil | |
| CN113621314A (en) | Solid polishing wax block based on modified rice bran wax and preparation method thereof | |
| CN113480943A (en) | Polishing wax oil based on modified rice bran wax and preparation method thereof | |
| CN111718390B (en) | Sterol cold precipitation formula liquid and application thereof | |
| CN113563805A (en) | High-gloss wax water based on modified rice bran wax and preparation method thereof | |
| CN113604156A (en) | Self-emulsifying wax oil based on modified rice bran wax and preparation method thereof | |
| SU447429A1 (en) | Continuous process for producing oxidized montan wax |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20211109 |