CN216777956U - Cosmetic grade 1,2 hexanediol purification device - Google Patents

Cosmetic grade 1,2 hexanediol purification device Download PDF

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CN216777956U
CN216777956U CN202123201274.1U CN202123201274U CN216777956U CN 216777956 U CN216777956 U CN 216777956U CN 202123201274 U CN202123201274 U CN 202123201274U CN 216777956 U CN216777956 U CN 216777956U
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tower
hdo
stripping
reboiler
light component
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李云旭
严瑾
陈多安
黄斌
王辉
李佳莉
胡海波
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Zhejiang Realsun Chemical Stock Co ltd
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Zhejiang Realsun Chemical Stock Co ltd
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Abstract

The utility model discloses a cosmetic grade 1,2 hexanediol purification device, and belongs to the technical field of fine chemical engineering. It comprises the following steps: the tower top of the stripping tower is filled with raw materials, and the tower bottom of the stripping tower is filled with steam and used for stripping the raw materials and then extracting primarily purified HDO; a light component removal column which is communicated with the stripping column and is used for removing light components in the primarily purified HDO; a fine distillation tower which is communicated with the lightness removing tower and is used for refining the HDO without light components into cosmetic-grade HDO; and the gas outlet end of the coupling heat exchange device is respectively connected with the light component removal tower and the fine steam tower and is used for heating the light component removal tower and the fine steam tower. The process of high-pressure steam stripping is adopted, impurities in the materials are removed in a steam entrainment mode, an entrainer or an adsorbent and the like do not need to be added, the follow-up produced product is ensured not to have peculiar smell which is difficult to remove, the whole purification process does not involve chemical reaction, the danger coefficient is low, the requirement on equipment is low, and the investment cost is reduced.

Description

Cosmetic grade 1,2 hexanediol purification device
Technical Field
The utility model belongs to the technical field of fine chemical engineering, and particularly relates to a cosmetic grade 1,2 hexanediol purification device.
Background
1, 2-Hexanediol (HDO) is an important chemical production raw material, and the excellent solubilizing ability of the HDO makes the HDO useful for producing color ink for an ink jet printer; is also an important organic synthesis intermediate, can produce 1, 2-adipic acid, amino alcohol and the like, and is used for high-grade coatings, high-grade glue, adhesives and the like; meanwhile, the preservative is a contactable preservative, has non-corrosive, bactericidal and moisturizing effects, can be used as a cosmetic additive, or can be added into perfume instead of alcohol, and has unusual expression in deodorant and antiperspirant.
With the increase of consumption level and the transformation of consumption concept, the scale of the cosmetic industry market is steadily increased in recent years, the sales increase of domestic cosmetics is steadily more than 10%, especially the high-end cosmetic market is continuously heated, and 1, 2-hexanediol is a commonly used humectant. High-end cosmetics have high requirements on the purity and smell of additives, the industrial grade 1, 2-hexanediol has low purity and has the smell similar to that of traditional Chinese medicines, the industrial grade HDO cannot be used as the high-end cosmetics additives, and the industrial grade HDO needs to be purified to be more than 99.9 percent and is odorless and tasteless.
The existing purification method of cosmetic grade 1, 2-hexanediol adopts a refining process of organic solvent extraction or activated carbon adsorption, but the method introduces organic impurities, has complex post-treatment process and higher production cost, and is difficult to remove the odor in HDO. Cosmetic-grade HDO is monopolized by foreign purification technology for a long time, and the prior domestic technology for removing the odor in the 1, 2-hexanediol still needs to be broken through.
For example, in the prior art, an invention patent with application number CN 202110074157.9 discloses 1, 2-hexanediol and a purification method thereof, 1-hexene is used as a raw material, 1, 2-hexanediol is prepared by epoxidation and hydrolysis, borohydride serving as an oxidant is added, low-temperature treatment is performed, and then reduced pressure distillation is performed, so that the purity of the obtained 1, 2-hexanediol product is 99%, and the obtained product has extremely low odor or no traditional Chinese medicine odor.
For example, an invention patent with application number KR101536934 in the prior art discloses a preparation method of high-purity 1, 2-hexanediol, which comprises the steps of mixing HDO with purity of 99.5% with water, adding sodium carbonate or sodium bicarbonate buffer solution for treatment, then carrying out reduced pressure distillation, activated carbon adsorption and filtration, deodorizing the product, further adding n-hexane solvent for treatment, carrying out reduced pressure distillation after layering, introducing high-purity nitrogen for bubbling treatment, and finally obtaining the high-purity 1, 2-hexanediol product. The obtained product has purity of 99.8%, water content of 0.2%, and no color or odor. However, the purification process has long flow, low efficiency and high operation requirement.
For example, an invention patent with application number KR 102038445B1 in the prior art discloses a method for purifying high-purity odorless 1, 2-hexanediol, and cosmetic-grade HDO is obtained through four-stage deodorization by deodorization, organic calcium carbonate removal, HDO recovery, two-stage deodorization, activated carbon adsorption, HDO recovery, three-stage deodorization, HDO recovery, four-stage deodorization and HDO recovery. The purification method has the advantages of complex process flow, high energy consumption and large equipment investment, and is not suitable for industrial production.
In conclusion, the purification device used in the traditional process for purifying the cosmetic grade 1, 2-hexanediol has the problems of complex purification process, higher operation requirement, difficulty in realizing continuous production and the like, and in addition, the problems of large investment and high energy consumption are caused by the need of adding an entrainer and/or an adsorbent and the involvement of chemical reaction.
Disclosure of Invention
Aiming at the problems in the prior art, the utility model provides a 1, 2-hexanediol purification device which has the advantages of small equipment investment, continuous production and capability of ensuring that the purified product can meet the cosmetic grade requirement.
The utility model can be realized by the following technical scheme:
a cosmetic grade 1,2 hexanediol purification apparatus, comprising:
the tower top of the stripping tower is filled with raw materials, and the tower bottom of the stripping tower is filled with steam and used for extracting primarily purified HDO after the raw materials are stripped;
a light component removal column in communication with the stripping column and configured to remove light components from the primarily purified HDO;
a fine distillation tower which is communicated with the lightness removing tower and is used for refining the HDO without light components into cosmetic-grade HDO;
and the gas inlet end of the coupling heat exchange device is connected with the stripping tower, and the gas outlet end of the coupling heat exchange device is respectively connected with the light component removal tower and the fine distillation tower and is used for heating the light component removal tower and the fine distillation tower.
As a further improvement of the present invention, the coupled heat exchange device comprises a steam recovery package, a first reboiler and a second reboiler, wherein a gas inlet end of the steam recovery package is connected to the top of the stripping column, and a gas outlet end of the steam recovery package is connected to the first reboiler and the second reboiler respectively.
In a further improvement of the present invention, both ends of the first reboiler are connected to the bottom of the light ends removal column, and both ends of the second reboiler are connected to the bottom of the finishing distillation column.
As a further improvement of the present invention, the system further comprises a first water cooler and a second water cooler, wherein both ends of the first reboiler are respectively connected to the steam recovery package and the first water cooler, and both ends of the second reboiler are respectively connected to the steam recovery package and the second water cooler.
As a further improvement of the utility model, the system further comprises a first condenser and a second condenser, wherein two ends of the first condenser are respectively connected with the tower top of the light component removal tower and an external vacuum unit, and two ends of the second condenser are respectively connected with the tower top of the fine distillation tower and the external vacuum unit.
As a further improvement of the utility model, the middle part of the lightness-removing column is connected with the tower kettle of the stripping column, and the middle part of the fine distillation column is connected with the tower kettle of the lightness-removing column.
Compared with the prior art, the utility model has the following beneficial effects:
1. the process of high-pressure steam stripping is adopted, impurities in the materials can be removed in a mode of carrying water vapor, an entrainer or an adsorbent and the like do not need to be added, and the follow-up produced product is ensured not to have peculiar smell which is difficult to remove.
2. The whole purification process does not involve chemical reaction, the danger coefficient is low, the requirement on equipment is lower, and the investment cost is reduced.
3. The stripping tower, the light component removal tower and the refining tower are used for coupling heat exchange, secondary steam generated by stripping is recycled, and energy loss in the production process is reduced.
Drawings
FIG. 1 is a process flow diagram of a cosmetic grade 1,2 hexanediol purification apparatus of the present invention.
In the figure, 100, a stripping tower; 110. a steam recovery package; 200. a light component removal tower; 210. a first reboiler; 220. a first water cooler; 230. a first condenser; 300. a fine distillation tower; 310. a second reboiler; 320. a second water cooler; 330. a second condenser; 400. a vacuum unit; 500. a booster pump.
Detailed Description
The following are specific embodiments of the present invention and the technical method of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
As shown in fig. 1, the present invention provides a cosmetic grade 1,2 hexanediol purification apparatus, comprising:
the stripping tower 100 is provided with raw materials and steam respectively entering the tower top and the tower bottom, and the steam strips the raw materials to obtain primarily purified HDO. Specifically, the stripping tower 100 is filled with high-pressure fresh steam, the steam is used as a medium to exchange with the material, secondary steam is discharged from the top of the stripping tower 100, and impurities in the HDO, which are difficult to remove by simple rectification, can be carried out along with the steam in an entrainment mode while the secondary steam is discharged, so that primarily purified HDO is obtained.
And the light component removal tower 200 is communicated with the stripping tower 100, and the primarily purified HDO can be rectified in the light component removal tower 200 to obtain the HDO with light components removed. Specifically, after the primarily purified HDO enters the light component removal tower 200, the light component removal tower 200 is rectified by a reduced pressure distillation method to obtain the HDO with light components removed.
And the fine distillation tower 300 is communicated with the lightness removing tower 200, and the HDO with the light components removed can be refined in the fine distillation tower 300 to extract the cosmetic-grade HDO. Specifically, after the HDO from which the light components are removed enters the fine distillation tower 300, the fine distillation tower 300 refines the HDO by way of rectification under reduced pressure, and finally a cosmetic-grade HDO product is obtained.
The gas inlet end of the coupling heat exchange device is connected with the stripping tower 100, the secondary steam discharged from the top of the stripping tower 100 firstly enters the coupling heat exchange device, and the gas outlet end of the coupling heat exchange device is respectively connected with the light component removal tower 200 and the refined distillation tower 300, so that the secondary steam entering the coupling heat exchange device can respectively heat the light component removal tower 200 and the refined distillation tower 300 after flowing out, the reutilization of the secondary steam is realized, the purpose of coupling heat exchange of the stripping tower 100, the light component removal tower 200 and the refined distillation tower is further realized, and the energy loss in the production process is reduced.
The purification device in the embodiment adopts a high-pressure steam stripping process, can remove impurities in materials in a steam entrainment mode, does not need an entrainer or an adsorbent and the like, ensures that the subsequent produced product does not have peculiar smell which is difficult to remove, and simultaneously does not relate to chemical reaction, so that the danger coefficient of the whole purification process is low, the requirement on equipment is lower, and the investment cost is reduced.
Preferably, the coupled heat exchange device comprises a steam recovery package 110, a first reboiler 210 and a second reboiler 310, wherein a gas inlet of the steam recovery package 110 is connected to the top of the stripping column 100, and a gas outlet of the steam recovery package 110 is connected to the first reboiler 210 and the second reboiler 310, respectively. The secondary steam generated at the top of the stripping tower 100 enters the steam recovery package 110, is divided into two parts, and enters the first reboiler 210 and the second reboiler 310 for reheating.
Preferably, both ends of the first reboiler 210 are connected to the bottom of the light ends removal column 200, and both ends of the second reboiler 310 are connected to the bottom of the finishing distillation column 300. Specifically, the first reboiler 210 and the second reboiler 310 are both installed on the tower body of the lightness-removing column 200 through a pipeline, so that the secondary steam entering the first reboiler 210 and the second reboiler 310 for reheating can exchange heat with the lightness-removing column 200 and the finishing distillation column 300 through a pipeline, and in the process, the secondary steam has high temperature, so that the reheating speed is high, and the temperatures of the lightness-removing column 200 and the finishing distillation column 300 can be quickly increased.
Preferably, the system further comprises a first water cooler 220 and a second water cooler 320, wherein both ends of the first reboiler 210 are connected to the steam recovery package 110 and the first water cooler 220, respectively, and both ends of the second reboiler 310 are connected to the steam recovery package 110 and the second water cooler 320, respectively. The first water cooler 220 is configured to condense and discharge secondary steam after heat exchange between the first reboiler 210 and the light component removal column 200, and similarly, the second water cooler 320 is configured to condense and discharge secondary steam after heat exchange between the second reboiler 310 and the finishing distillation column 300.
Preferably, the system further comprises a first condenser 230 and a second condenser 330, two ends of the first condenser 230 are respectively connected with the top of the light component removal tower 200 and the external vacuum unit 400, two ends of the second condenser 330 are respectively connected with the top of the finishing distillation tower 300 and the external vacuum unit 400, wherein the vacuum unit 400 is configured to provide a vacuum environment for the vacuum distillation process of the light component removal tower 200 and the vacuum distillation process of the finishing distillation tower 300.
Specifically, after the primarily purified HDO in the light component removal tower 200 is subjected to pressure reduction and light component removal, the HDO with the light component removed is obtained and discharged from the tower kettle of the light component removal tower 200 to enter the fine distillation tower 300, at this time, the removed light component enters the first condenser 230 from the tower top of the light component removal tower 200 to be condensed, and the condensed liquid material partially flows back to the light component removal tower 200, and the rest is output; the HDO removed with light components entering the rectifying tower 300 can be extracted from the top of the rectifying tower 300 after being subjected to reduced pressure rectification, enters the second condenser 330 for condensation, a part of cosmetic-grade HDO can be obtained after the condensation, the rest of cosmetic-grade HDO flows back into the rectifying tower 300, and the heavy components are extracted from the tower kettle of the rectifying tower 300.
Preferably, the raw crude HDO is fed from the top of the stripping tower 100 through a feeding pump, the primarily purified HDO extracted from the bottom of the stripping tower 100 is pressurized by a pressurizing pump 500 and fed from the middle of the light component removal tower 200, and the HDO removed from the bottom of the light component removal tower 200 is fed from the middle of the fine distillation tower 300.
The technical means disclosed by the scheme of the utility model are not limited to the technical means disclosed by the technical means, and the technical scheme also comprises the technical scheme formed by any combination of the technical characteristics. The foregoing is a detailed description of the utility model, and it should be noted that modifications and adaptations can be made by those skilled in the art without departing from the principle of the utility model, and are intended to be within the scope of the utility model.
It should be noted that all the directional indicators (such as up, down, left, right, front, and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
Moreover, descriptions of the present invention as relating to "first," "second," "a," etc. are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicit ly indicating a number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, four, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "connected," "secured," and the like are to be construed broadly, and for example, "secured" may be a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.

Claims (6)

1. A cosmetic grade 1,2 hexanediol purification apparatus, comprising:
the tower top of the stripping tower is filled with raw materials, and the tower bottom of the stripping tower is filled with steam and used for extracting primarily purified HDO after the raw materials are stripped;
a light component removal column in communication with the stripping column and configured to remove light components from the primarily purified HDO;
a fine distillation tower which is communicated with the lightness removing tower and is used for refining the HDO without light components into cosmetic-grade HDO;
and the gas inlet end of the coupling heat exchange device is connected with the stripping tower, and the gas outlet end of the coupling heat exchange device is respectively connected with the light component removal tower and the fine distillation tower and is used for heating the light component removal tower and the fine distillation tower.
2. The apparatus of claim 1, wherein the coupled heat exchanger comprises a steam recovery package, a first reboiler, and a second reboiler, wherein an inlet of the steam recovery package is connected to the top of the stripping tower, and an outlet of the steam recovery package is connected to the first reboiler and the second reboiler, respectively.
3. The apparatus for purifying 1, 2-hexanediol as set forth in claim 2, wherein both ends of the first reboiler are connected to the bottom of the light component removal column, and both ends of the second reboiler are connected to the bottom of the distillation column.
4. The apparatus of claim 2, further comprising a first water cooler and a second water cooler, wherein the first reboiler is connected to the steam recovery package and the first water cooler, and the second reboiler is connected to the steam recovery package and the second water cooler.
5. The device for purifying the cosmetic grade 1, 2-hexanediol according to claim 1, further comprising a first condenser and a second condenser, wherein two ends of the first condenser are respectively connected with the top of the light component removal tower and an external vacuum unit, and two ends of the second condenser are respectively connected with the top of the fine distillation tower and the external vacuum unit.
6. The apparatus for purifying 1, 2-hexanediol as a cosmetic grade according to claim 1, wherein the middle part of the lightness-removing column is connected to the bottom of the stripping column, and the middle part of the finishing distillation column is connected to the bottom of the lightness-removing column.
CN202123201274.1U 2021-12-17 2021-12-17 Cosmetic grade 1,2 hexanediol purification device Active CN216777956U (en)

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CN202123201274.1U CN216777956U (en) 2021-12-17 2021-12-17 Cosmetic grade 1,2 hexanediol purification device

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Application Number Priority Date Filing Date Title
CN202123201274.1U CN216777956U (en) 2021-12-17 2021-12-17 Cosmetic grade 1,2 hexanediol purification device

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Publication Number Publication Date
CN216777956U true CN216777956U (en) 2022-06-21

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