CN107986957A - A kind of preparation method of sorbic acid - Google Patents
A kind of preparation method of sorbic acid Download PDFInfo
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- CN107986957A CN107986957A CN201711287299.3A CN201711287299A CN107986957A CN 107986957 A CN107986957 A CN 107986957A CN 201711287299 A CN201711287299 A CN 201711287299A CN 107986957 A CN107986957 A CN 107986957A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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Abstract
The invention belongs to chemical production field, and in particular to a kind of preparation method of sorbic acid.In the aqueous solution for the ethanol that sorbic acid crude product after decoloration is dissolved in, concentration of the sorbic acid in ethanol solution is 15~30%, and heating stirring, temperature control forms the supersaturated solution of sorbic acid at 45~60 DEG C；The supersaturated solution is interior when 1~5 is small, and temperature is slowly dropped to 25~40 DEG C, and afterwards, 1~6 is interior when small, is slowly dropped to 5~20 DEG C, sorbic acid crystals are obtained by filtration.The sorbic acid prepared using present invention process scheme, is efficiently separated sorb acid isomer, does not detect isomers, and HPLC contents reach more than 99.9%.
Description
Technical field
The invention belongs to chemical production field, and in particular to a kind of preparation method of high-quality sorbic acid.
Background technology
Sorbic acid, also known as：2,4- hexadienoic acids, white needles or powdered crystal；Water is slightly soluble in, can be dissolved in a variety of organic
Solvent；Molecular weight：112.13, fusing point：132-135 DEG C, boiling point：228 DEG C (decomposition), density：1.204(19℃).Sorbic acid is
A kind of to have the unrighted acid for gripping diene altogether, it can effectively inhibit the activity of mould, saccharomycete and aerobic bacteria, its
It is more stronger than bactericidal effect to suppress the effect of harmful microorganism development and breeding, is that Food and Drug Administration is recommended to countries in the world
Preservative, its security are two times of salt.Sorbic acid is widely used to various food, veterinary antibiotics, medicine, rubber, makes
The anti-corrosion of the industries such as paper, animal feed, cosmetics, paint, tobacco, beverage and fresh-keeping.
It is industrial at present that sorbic acid is prepared using hydrochloric acid hydrolysis sorbic acid polyester more.In polyester hydrolytic process, 4 kinds are produced
2,4- hexadienoic acid isomers, wherein only anti-, trans- 2,4- hexadienoic acids are target product sorbic acid, and hydrolysis is selective
For 80%~92%, remaining 8%~20% is other 3 kinds of isomers, high polymer and other by-products, through decoloration, is removed most of
Isomers, high polymer and other by-products, obtain sorbic acid crude product, obtain sorb acid product after refined, are detected through HPLC, content is about
99.5%, and have a small amount of isomers, and high-end customer requires HPLC contents to reach more than 99.9%.Therefore my company have developed one
The preparation method of kind high-quality sorbic acid.
After the method for refined sorbic acid crude product industrial at present is mainly using organic solvent rising temperature for dissolving such as alcohols, directly
Crystallisation by cooling, is washed through deionized water again after separation, dry sorbic acid finished product.Such technological operation is simple, but sorbic acid is pure
Change degree is not high, and there are a small amount of isomers.
The content of the invention
To solve the above-mentioned problems, it is an object of the invention to provide providing a kind of preparation process of high-quality sorbic acid,
Sorb acid isomer is efficiently separated, sorbic acid finished product HPLC contents reach more than 99.9%.
Technical scheme is as follows：
(concentration of the sorbic acid in ethanol solution is in the aqueous solution for the ethanol that sorbic acid crude product after decoloration is dissolved in
15~30%), heating stirring, temperature control is at 45~60 DEG C, preferably 48~55 DEG C, forms the supersaturated solution of sorbic acid, should
Supersaturated solution 1~5 is interior when small, and temperature is slowly dropped to 25~40 DEG C, and afterwards, 1~6 is interior when small, is slowly dropped to 5~20 DEG C.Cross
Filter obtains sorbic acid crystals.Sorbic acid prepared by the technique does not detect isomers, and sorbic acid HPLC contents are more than 99.9%.
Further, the volumetric concentration of the ethanol water is 30%~60%, the volume of further ethanol water
Concentration is 40%~50%.
Further, the content that the sorbic acid crude product is is 80-92%.
The preparation method of a kind of sorbic acid according to the present invention, the obtained sorbic acid crystals HPLC contents are more than
99.9%.
The preparation method of a kind of sorbic acid according to the present invention, it is preferred that the supersaturated solution is when 1~2 is small
Interior, temperature is slowly dropped to 25~40 DEG C, and afterwards, 1~6 is interior when small, is slowly dropped to 5~20 DEG C.
The preparation method of a kind of sorbic acid according to the present invention, it is preferred that the supersaturated solution is when 3~4 is small
Interior, temperature is slowly dropped to 30~40 DEG C, and afterwards, 4~5 is interior when small, is slowly dropped to 10~20 DEG C.
The preparation method of a kind of sorbic acid according to the present invention, it is further preferred that, the supersaturated solution 4~
5 is interior when small, and temperature is slowly dropped to 25~30 DEG C, and afterwards, 5~6 is interior when small, is slowly dropped to 5~10 DEG C.
For in sorbic acid subtractive process, sorbic acid purification effect is bad.The present invention is used using ethanol as solvent, carries out ladder
The method of decrease temperature crystalline is spent, utilizes the solubility and dissolving speed of sorbic acid during decrease temperature crystalline and isomers in ethanol solution
The difference of degree, controls suitable cooling rate, makes sorbic acid solutions all the time in metastable state and maintains suitable degree of supersaturation,
So that the sorbic acid crystals purity separated out is higher.
Beneficial effects of the present invention are as follows：
A kind of preparation method of sorbic acid provided by the invention, is more than 99.9% using this technique sorbic acid HPLC contents,
Technological operation is simple, and sorbic acid not easily runs off, and solvent easily recycles.
Embodiment
With reference to embodiment, the present invention is further elaborated, it will be appreciated by those skilled in the art that the embodiment
It is given for example only, without forming any restrictions to the present invention.
Embodiment 1：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 550g30%, is added,
Heating stirring, is heated to 50 DEG C, interior when 2 is small to be at the uniform velocity cooled to 40 DEG C, interior when 5 is small to be at the uniform velocity cooled to 20 DEG C, is obtained by filtration
Sorbic acid crystals, liquid chromatography (HPLC) measure Determination of sorbic 99.92%.
Embodiment 2：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 300g30%, is added,
60 DEG C are heated to, it is interior when 5 is small to be at the uniform velocity cooled to 30 DEG C, it is interior when 6 is small to be at the uniform velocity cooled to 10 DEG C, sorb acid crystals is obtained by filtration
Body, liquid chromatography (HPLC) measure Determination of sorbic 99.91%.
Embodiment 3：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution for, adding 550g40% adds
Heat to 48 DEG C it is interior when 1 is small be at the uniform velocity cooled to 40 DEG C, it is interior when 6 is small to be at the uniform velocity cooled to 5 DEG C, sorbic acid crystals, liquid is obtained by filtration
Phase chromatography (HPLC) measures Determination of sorbic 99.92%.
Embodiment 4：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 300g40%, is added,
Heating stirring, is heated to 55 DEG C, interior when 3 is small to be at the uniform velocity cooled to 40 DEG C, interior when 6 is small to be at the uniform velocity cooled to 20 DEG C, is obtained by filtration
Sorbic acid crystals, liquid chromatography (HPLC) measure Determination of sorbic 99.91%.
Embodiment 5：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 400g50%, is added,
50 DEG C are heated to, it is interior when 4 is small to be at the uniform velocity cooled to 40 DEG C, it is interior when 4 is small to be at the uniform velocity cooled to 20 DEG C, sorb acid crystals is obtained by filtration
Body, liquid chromatography (HPLC) measure Determination of sorbic 99.93%.
Embodiment 6：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 230g50%, is added,
55 DEG C are heated to, it is interior when 4 is small to be at the uniform velocity cooled to 30 DEG C, it is interior when 5 is small to be at the uniform velocity cooled to 10 DEG C, sorb acid crystals is obtained by filtration
Body, liquid chromatography (HPLC) measure Determination of sorbic 99.93%.
Embodiment 7：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 550g60%, is added,
45 DEG C are heated to, it is interior when 1 is small to be at the uniform velocity cooled to 25 DEG C, it is interior when 1 is small to be at the uniform velocity cooled to 5 DEG C, sorbic acid crystals are obtained by filtration,
Liquid chromatography (HPLC) measures Determination of sorbic 99.92%.
Embodiment 8：
A kind of sorbic acid waste acidity recovery treatment process, comprises the following steps：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 230g60%, is added,
Be heated to 50 DEG C, 5 it is interior when small be at the uniform velocity cooled to 25 DEG C, it is interior when 6 is small to be at the uniform velocity cooled to 5 DEG C, sorb acid crystals is obtained by filtration
Body, liquid chromatography (HPLC) measure Determination of sorbic 99.94%.
Comparative example：
Thick sorbic acid (the contents of 100g are added in 1000ml beakers：90.21%) ethanol solution of 400g40%, is added,
It is heated to, 70 DEG C, it is interior when 10 is small to be at the uniform velocity cooled to 15 DEG C, sorbic acid crystals are obtained by filtration, liquid chromatography (HPLC) measures
Determination of sorbic 99.86%.
The present invention is disclosed with preferred embodiment above, so it is not intended to limiting the invention, all to use equivalent substitution
Or the technical solution that equivalent transformation mode is obtained, it is within the scope of the present invention.
Claims (7)
1. a kind of preparation method of sorbic acid, it is characterised in that include the following steps：Sorbic acid crude product after decoloration is dissolved in
Ethanol aqueous solution in, concentration of the sorbic acid in ethanol solution be 15~30%, heating stirring, temperature control is 45~60
DEG C, form the supersaturated solution of sorbic acid；The supersaturated solution is interior when 1~5 is small, and temperature is slowly dropped to 25~40 DEG C, it
Afterwards, it is interior when 1~6 is small, 5~20 DEG C are slowly dropped to, sorbic acid crystals are obtained by filtration.
2. a kind of preparation method of sorbic acid according to claim 1, it is characterised in that the volume of the ethanol water is dense
Spend for 30%~60%.
A kind of 3. preparation method of sorbic acid according to claim 1, it is characterised in that the content that the sorbic acid crude product is
For 80-92%.
A kind of 4. preparation method of sorbic acid according to claim 1, it is characterised in that the obtained sorbic acid crystals
HPLC contents are more than 99.9%.
5. a kind of preparation method of sorbic acid according to claim 1, it is characterised in that the supersaturated solution is small 1~2
When it is interior, temperature is slowly dropped to 25~40 DEG C, and afterwards, 1~6 is interior when small, is slowly dropped to 5~20 DEG C.
6. a kind of preparation method of sorbic acid according to claim 1, it is characterised in that the supersaturated solution is small 3~4
When it is interior, temperature is slowly dropped to 30~40 DEG C, and afterwards, 4~5 is interior when small, is slowly dropped to 10~20 DEG C.
7. a kind of preparation method of sorbic acid according to claim 1, it is characterised in that the supersaturated solution is small 4~5
When it is interior, temperature is slowly dropped to 25~30 DEG C, and afterwards, 5~6 is interior when small, is slowly dropped to 5~10 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711287299.3A CN107986957A (en) | 2017-12-07 | 2017-12-07 | A kind of preparation method of sorbic acid |
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| CN201711287299.3A CN107986957A (en) | 2017-12-07 | 2017-12-07 | A kind of preparation method of sorbic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642698A (en) * | 2019-10-31 | 2020-01-03 | 江苏润普食品科技股份有限公司 | Production method for preparing sorbic acid by acidolysis of sorbic acid polyester |
| CN115010595A (en) * | 2022-07-27 | 2022-09-06 | 江苏道尔顿石化科技有限公司 | Method for forming crude crystals of sorbic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377874A (en) * | 2002-04-12 | 2002-11-06 | 浙江大学 | Process for preparing sorbic acid |
| CN101928307A (en) * | 2010-08-24 | 2010-12-29 | 安徽省皖北药业股份有限公司 | Crystallization method of clindamycin phosphate |
| CN104788307A (en) * | 2015-05-04 | 2015-07-22 | 湖南尔康制药股份有限公司 | Method for purifying sorbic acid |
-
2017
- 2017-12-07 CN CN201711287299.3A patent/CN107986957A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1377874A (en) * | 2002-04-12 | 2002-11-06 | 浙江大学 | Process for preparing sorbic acid |
| CN101928307A (en) * | 2010-08-24 | 2010-12-29 | 安徽省皖北药业股份有限公司 | Crystallization method of clindamycin phosphate |
| CN104788307A (en) * | 2015-05-04 | 2015-07-22 | 湖南尔康制药股份有限公司 | Method for purifying sorbic acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642698A (en) * | 2019-10-31 | 2020-01-03 | 江苏润普食品科技股份有限公司 | Production method for preparing sorbic acid by acidolysis of sorbic acid polyester |
| CN115010595A (en) * | 2022-07-27 | 2022-09-06 | 江苏道尔顿石化科技有限公司 | Method for forming crude crystals of sorbic acid |
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Application publication date: 20180504 |