CN117402348A - Preparation method of sorbitol polyether-30 tetraoleate - Google Patents
Preparation method of sorbitol polyether-30 tetraoleate Download PDFInfo
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- CN117402348A CN117402348A CN202311227995.0A CN202311227995A CN117402348A CN 117402348 A CN117402348 A CN 117402348A CN 202311227995 A CN202311227995 A CN 202311227995A CN 117402348 A CN117402348 A CN 117402348A
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- Prior art keywords
- parts
- reaction
- sorbitol polyether
- decoloring
- tetraoleate
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Links
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 title claims abstract description 38
- 239000000600 sorbitol Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005886 esterification reaction Methods 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 18
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 18
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005642 Oleic acid Substances 0.000 claims abstract description 18
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 18
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000032050 esterification Effects 0.000 abstract description 4
- 150000002148 esters Chemical class 0.000 abstract description 4
- 239000010865 sewage Substances 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000004821 distillation Methods 0.000 abstract description 2
- 239000002932 luster Substances 0.000 abstract description 2
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000002253 acid Substances 0.000 description 5
- 230000001804 emulsifying effect Effects 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 239000006071 cream Substances 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 241001550224 Apha Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Classifications
-
- 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
Abstract
The invention relates to a preparation method of sorbitol polyether-30 tetraoleate. The invention adopts the steps of esterification reaction synthesis of sorbitol polyether-30 and oleic acid under the presence of an organotin catalyst, and the whole production process comprises the steps of esterification, reduced pressure distillation, decoloration and the like, so as to prepare the sorbitol polyether-30 tetraoleate; the preparation method uses the catalyst organotin, can shorten the esterification period, can recycle the catalyst, improves the conversion rate, reduces the production cost, and simultaneously has light color and luster of the ester product, high quality, no need of post-treatment such as neutralization, alkali washing, water washing and the like in the reaction process, and also avoids equipment corrosion, i.e. no sewage discharge and no sewage treatment cost, thereby saving water resources and not polluting the environment.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to a preparation method of sorbitol polyether-30 tetraoleate.
Background
The sorbitol polyether-30 tetraoleate is an ester derivative, and is a nonionic surfactant with an emulsifying effect. It can be derived from plants and is biodegradable; has excellent emulsifying property, can be prepared into a stable emulsifying system with a small amount of oil and grease, can be used as an emulsifying agent in the oil-in-water reaction process, and can be used for removing oil and the like, and is suitable for emulsifying polar and nonpolar oil. Good compatibility with oil agent, excellent solubility, and can dissolve vegetable oil and synthetic ester, thereby improving the stability of the product. The cleansing cream has strong cleansing ability and good cleansing effect, is also suitable for cleansing thick cosmetics, and can be used in cream, moisturizing cream and milk.
Because of the wide application of the products, the demand is continuously increased, and the production and preparation methods of the products are required to be continuously improved, so that the production efficiency is improved, the production cost is reduced, and the requirement of environmental protection is met.
Disclosure of Invention
In view of the problems existing in the prior art, the invention discloses a preparation method of sorbitol polyether-30 tetraoleate, which comprises the following steps:
step one, preparing raw materials: taking, by mass, 30 1400-1600 parts of sorbitol polyether, 900-1200 parts of oleic acid, 12-15 parts of an organotin catalyst and 12-17 parts of a decoloring agent;
step two, esterification reaction: adding sorbitol polyether-30, oleic acid and an organotin catalyst which are taken according to parts by weight into a reaction kettle, fully and uniformly stirring, and then carrying out esterification reaction, and stopping the esterification reaction when the sampled acid value is less than 1mgKOH/g to obtain an initial mixture;
step three, collecting moisture: collecting water generated in the second step through a reflux water separator arranged in the reaction kettle, cooling and separating a water layer, and then returning the water to the reaction kettle for continuous reaction;
step four, decoloring: adding the initial mixture, the decoloring agent and the decoloring auxiliary agent into a decoloring kettle, stirring, controlling the temperature to be 110-120 ℃, performing reduced pressure adsorption decoloring, stirring for 30 minutes, cooling, filtering and discharging to obtain the sorbitol polyether-30 tetraoleate.
As a preferable scheme of the invention, the esterification reaction in the second step is divided into two esterification reactions, namely a first esterification reaction in which the temperature is raised to 130-140 ℃ and the reaction time is 1-2.5 hours, and a second esterification reaction in which the temperature is raised to 175-180 ℃ and the reaction time is 3-5 hours under the condition of gradually vacuumizing and adjusting to-0.04 MPa, so that the mixture of the organotin catalyst, the sorbitol polyether-30 and the oleic acid is fully reacted in a reaction kettle.
The invention has the beneficial effects that: the invention adopts the steps of esterification reaction synthesis of sorbitol polyether-30 and oleic acid under the presence of an organotin catalyst, and the whole production process comprises the steps of esterification, reduced pressure distillation, decoloration and the like, so as to prepare the sorbitol polyether-30 tetraoleate; the preparation method uses the catalyst organotin, can shorten the esterification period, can recycle the catalyst, improves the conversion rate, reduces the production cost, and simultaneously has light color and luster of the ester product, high quality, no need of post-treatment such as neutralization, alkali washing, water washing and the like in the reaction process, and also avoids equipment corrosion, i.e. no sewage discharge and no sewage treatment cost, thereby saving water resources and not polluting the environment.
Detailed Description
Example 1
The invention relates to a preparation method of sorbitol polyether-30 tetraoleate, which comprises the following steps:
step one, preparing raw materials: taking, by mass, 30 1400 parts of sorbitol polyether, 900 parts of oleic acid, 12 parts of an organotin catalyst and 12 parts of a decoloring agent;
step two, esterification reaction: adding sorbitol polyether-30, oleic acid and an organotin catalyst which are taken according to parts by weight into a reaction kettle, fully stirring uniformly, and then carrying out esterification reaction, wherein the esterification reaction is divided into two times of esterification reaction, namely, a first time of esterification reaction which is carried out at the temperature of up to 130 ℃ and the reaction time of 1 hour, and a second time of esterification reaction which is carried out at the temperature of up to 175 ℃ and the reaction time of 3 hours under the condition of gradually vacuumizing and adjusting to-0.04 MPa, so that the mixture of the organotin catalyst, the sorbitol polyether-30 and the oleic acid fully reacts in the reaction kettle, and after the acid value of a sample is less than 1mgKOH/g, terminating the esterification reaction to obtain an initial mixture;
step three, collecting moisture: collecting water generated in the second step through a reflux water separator arranged in the reaction kettle, cooling and separating a water layer, and then returning the water to the reaction kettle for continuous reaction;
step four, decoloring: adding the initial mixture, the decoloring agent and the decoloring auxiliary agent into a decoloring kettle, stirring, controlling the temperature at 110 ℃, performing reduced pressure adsorption decoloring, cooling after stirring for 30 minutes, filtering and discharging to obtain the sorbitol polyether-30 tetraoleate.
Example 2
The invention relates to a preparation method of sorbitol polyether-30 tetraoleate, which comprises the following steps:
step one, preparing raw materials: taking, by mass, 30 1600 parts of sorbitol polyether, 1200 parts of oleic acid, 15 parts of an organotin catalyst and 17 parts of a decoloring agent;
step two, esterification reaction: adding sorbitol polyether-30, oleic acid and an organotin catalyst which are taken according to parts by weight into a reaction kettle, fully stirring uniformly, and then carrying out esterification reaction, wherein the esterification reaction is divided into two times of esterification reaction, namely, a first time of esterification reaction with the reaction time of 2.5 hours at the temperature of up to 140 ℃, and a second time of esterification reaction with the reaction time of 5 hours at the temperature of up to 180 ℃ under the condition of gradually vacuumizing and adjusting to-0.04 MPa, so that the mixture of the organotin catalyst, the sorbitol polyether-30 and the oleic acid fully reacts in the reaction kettle, and stopping the esterification reaction after the sampled acid value is less than 1mgKOH/g, thereby obtaining an initial mixture;
step three, collecting moisture: collecting water generated in the second step through a reflux water separator arranged in the reaction kettle, cooling and separating a water layer, and then returning the water to the reaction kettle for continuous reaction;
step four, decoloring: adding the initial mixture, the decoloring agent and the decoloring auxiliary agent into a decoloring kettle, stirring, controlling the temperature at 120 ℃, performing reduced pressure adsorption decoloring, cooling after stirring for 30 minutes, filtering and discharging to obtain the sorbitol polyether-30 tetraoleate.
Example 3
The invention relates to a preparation method of sorbitol polyether-30 tetraoleate, which comprises the following steps:
step one, preparing raw materials: taking, by mass, 30 1500 parts of sorbitol polyether, 1000 parts of oleic acid, 13.5 parts of an organotin catalyst and 15 parts of a decoloring agent;
step two, esterification reaction: adding sorbitol polyether-30, oleic acid and an organotin catalyst which are taken according to parts by weight into a reaction kettle, fully stirring uniformly, and then carrying out esterification reaction, wherein the esterification reaction is divided into two times of esterification reaction, namely, a first time of esterification reaction with the reaction time of 2 hours at the temperature of up to 135 ℃, gradually vacuumizing and adjusting to-0.04 MPa, and a second time of esterification reaction with the reaction time of up to 178 ℃, so that the mixture of the organotin catalyst, the sorbitol polyether-30 and the oleic acid fully reacts in the reaction kettle, and stopping the esterification reaction after the acid value of the sample is less than 1mgKOH/g, thereby obtaining an initial mixture;
step three, collecting moisture: collecting water generated in the second step through a reflux water separator arranged in the reaction kettle, cooling and separating a water layer, and then returning the water to the reaction kettle for continuous reaction;
step four, decoloring: adding the initial mixture, the decoloring agent and the decoloring auxiliary agent into a decoloring kettle, stirring, controlling the temperature at 115 ℃, performing reduced pressure adsorption decoloring, cooling after stirring for 30 minutes, filtering and discharging to obtain the sorbitol polyether-30 tetraoleate.
The main technical indexes of the obtained sorbitol polyether-30 tetraoleate are as follows:
| project | Unit (B) | Standard requirements |
| Appearance of | - | Colorless or pale yellow transparent liquid |
| Chromaticity of | APHA | 0-50 |
| Acid value | mgKOH/g | 0-5 |
| Saponification value | mgKOH/g | 70-100 |
| Iodine value | g/100g | 0-1 |
| Moisture content | ％ | 0-0.5 |
The components not described in detail herein are prior art.
Although the specific embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes and modifications without inventive labor may be made within the scope of the present invention without departing from the spirit of the present invention, which is within the scope of the present invention.
Claims (3)
1. The preparation method of the sorbitol polyether-30 tetraoleate is characterized by comprising the following steps:
step one, preparing raw materials: taking, by mass, 30 1400-1600 parts of sorbitol polyether, 900-1200 parts of oleic acid, 12-15 parts of an organotin catalyst and 12-17 parts of a decoloring agent;
step two, esterification reaction: adding sorbitol polyether-30, oleic acid and an organotin catalyst which are taken according to parts by weight into a reaction kettle, and fully and uniformly stirring to perform esterification reaction to obtain an initial mixture;
step three, collecting moisture: collecting water generated in the second step through a reflux water separator arranged in the reaction kettle, cooling and separating a water layer, and then returning the water to the reaction kettle for continuous reaction;
step four, decoloring: adding the initial mixture, the decoloring agent and the decoloring auxiliary agent into a decoloring kettle, stirring, controlling the temperature to be 110-120 ℃, performing reduced pressure adsorption decoloring, stirring for 30 minutes, cooling, filtering and discharging to obtain the sorbitol polyether-30 tetraoleate.
2. The method for preparing sorbitol polyether-30 tetraoleate according to claim 1, wherein: the first step comprises the following raw materials in parts by mass: sorbitol polyether-30 1500 parts, oleic acid 1000 parts, an organotin catalyst 13.5 parts and a decoloring agent 15 parts.
3. The method for preparing sorbitol polyether-30 tetraoleate according to claim 1, wherein: the esterification reaction is divided into two times, namely a first esterification reaction with the temperature increased to 130-140 ℃ and the reaction time of 1-2.5 hours, and a second esterification reaction with the temperature increased to 175-180 ℃ and the reaction time of 3-5 hours under the condition of gradually vacuumizing and adjusting to-0.04 MPa, so that the mixture of the organotin catalyst and the sorbitol polyether-30 and the oleic acid fully reacts in the reaction kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311227995.0A CN117402348A (en) | 2023-09-22 | 2023-09-22 | Preparation method of sorbitol polyether-30 tetraoleate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311227995.0A CN117402348A (en) | 2023-09-22 | 2023-09-22 | Preparation method of sorbitol polyether-30 tetraoleate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117402348A true CN117402348A (en) | 2024-01-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311227995.0A Pending CN117402348A (en) | 2023-09-22 | 2023-09-22 | Preparation method of sorbitol polyether-30 tetraoleate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117402348A (en) |
-
2023
- 2023-09-22 CN CN202311227995.0A patent/CN117402348A/en active Pending
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