CN114568588A - Inclusion or coated benzoic acid for feed and preparation method thereof - Google Patents
Inclusion or coated benzoic acid for feed and preparation method thereof Download PDFInfo
- Publication number
- CN114568588A CN114568588A CN202210213791.0A CN202210213791A CN114568588A CN 114568588 A CN114568588 A CN 114568588A CN 202210213791 A CN202210213791 A CN 202210213791A CN 114568588 A CN114568588 A CN 114568588A
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- benzoic acid
- inclusion
- coating
- cyclodextrin
- feed
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/111—Aromatic compounds
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/163—Sugars; Polysaccharides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Animal Husbandry (AREA)
- Medicinal Preparation (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of feed additive synthesis, and particularly relates to a novel inclusion or coated benzoic acid green preparation process. The green preparation process of the inclusion or coating benzoic acid comprises the steps of carrying out inclusion on feed-grade benzoic acid and cyclodextrin aqueous solution to form inclusion or coating benzoic acid solution, and carrying out spray drying to prepare the novel inclusion or coating benzoic acid. The invention overcomes the defects of large pungent smell, large esophagus and stomach irritation, poor animal edibility, poor bacteriostatic and antibacterial effects and the like when the traditional feed-grade benzoic acid is added for use. The novel inclusion or coating of the benzoic acid is convenient to use, reduces the pungent smell of the benzoic acid, improves the palatability, enables the feed to be eaten by animals, improves the feed utilization rate, avoids the irritation of the benzoic acid in esophagus or stomach, enables the benzoic acid to be continuously released in intestinal tracts, and plays a long-acting sterilization and bacteriostasis effect. The green preparation process has the advantages of mild reaction conditions, high reaction efficiency, no three wastes, simple and advanced process and suitability for industrial production of the feed.
Description
Technical Field
The invention belongs to the technical field of feed additive synthesis, and particularly relates to a novel inclusion or coated benzoic acid green preparation method.
Background
Benzoic acid, also known as benzoic acid, with molecular formula C6H5COOH, the simplest aromatic acid in which the carboxyl group is directly attached to a carbon atom of a benzene ring, is a compound in which one hydrogen atom of the benzene ring is replaced with a carboxyl group (-COOH). Is colorless and odorless flaky crystal. Slightly soluble in water, and easily soluble in organic solvents such as ethanol, diethyl ether, chloroform, benzene, toluene, carbon disulfide, carbon tetrachloride and turpentine. In the form of the free acid, ester or derivative thereof, are widely found in nature.
Disclosure of Invention
When the traditional feed-grade benzoic acid is added for use, the defects of strong pungent smell, strong esophagus and stomach irritation and the like exist; resulting in poor animal edibility and poor bacteriostatic and antibacterial effects. In order to solve the existing defects, the invention provides a green cyclodextrin inclusion or coating preparation process. The prepared inclusion or coating benzoic acid reduces the pungent smell of benzoic acid, improves the palatability, enables the feed to be eaten by animals and improves the utilization rate of the feed; the irritation of benzoic acid in esophagus or stomach is avoided, the benzoic acid is released in intestinal tract continuously, and the long-acting sterilization and bacteriostasis effects are achieved.
The green preparation process has the advantages of mild reaction conditions, high reaction efficiency, no three wastes, simple and advanced process and suitability for industrial production of the feed.
The green preparation process includes coating feed level benzoic acid and cyclodextrin aqua to form inclusion or coated benzoic acid solution, and spray drying to obtain new inclusion or coated benzoic acid.
The inclusion or coating benzoic acid green preparation process includes the following specific steps.
(1) Adding 5-30 parts of pure water into a reaction kettle, heating to 40-100 ℃, starting stirring, and adding 1-5 parts of cyclodextrin into the pure water in batches; stirring and dissolving evenly for later use. Preferably, the pure water amount: 10-20 parts of, heating temperature: 60-80 ℃, cyclodextrin content: 1-2 parts.
(2) And (2) dropwise adding 0.1-2 parts of benzoic acid ethanol solution (benzoic acid: 95% ethanol mass ratio =1: 2-4) into the reaction system in the step (1), and after dropwise adding, carrying out heat preservation reaction for 1-4 hours. Preferably: ethanol solution of benzoic acid: 0.5-1 part, the mass ratio of benzoic acid to 95% ethanol =1: 2, the heat preservation temperature: and (3) keeping the temperature at 60-80 ℃, and reacting for a time: 2-3 hours.
(3) And (3) carrying out pressure filtration on the reaction liquid obtained in the step (2) while the reaction liquid is hot, and then carrying out spray drying to obtain inclusion or coated benzoic acid powder.
The cyclodextrin in the step (1) is one or more of alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin, hydroxypropyl-beta-cyclodextrin, methyl-beta-cyclodextrin and sulfobutyl-beta-cyclodextrin.
The spray drying in the step (3) is to rapidly dry the inclusion or coating benzoic acid solution, and the spray drying conditions are as follows: feeding temperature: 100-200 ℃, flow rate of a feed pump: 5-50L/h, discharge temperature: 50 to 100 ℃. Preferably: feeding temperature: 120-150 ℃, flow rate of a feed pump: 20-30L/h, discharge temperature: 70-80 ℃.
The present invention will be further described with reference to the following examples.
Example 1.
Adding 1000kg of pure water into a reaction kettle, heating to 70 ℃, starting stirring, and adding 100kg of alpha-cyclodextrin into the pure water in batches; stirring and dissolving. 150kg of benzoic acid ethanol solution (50 kg of benzoic acid is dissolved in 100kg of 95% ethanol in advance) is added dropwise, and the temperature is kept for reaction for 2 hours. Then the reaction solution was subjected to pressure filtration while it was hot and spray-dried (spray-drying conditions: feed temperature: 150 ℃, feed pump flow rate: 30L/h, discharge temperature: 80 ℃) to obtain 142kg of inclusion or coated benzoic acid powder. Yield: 94.7 percent. Content of benzoic acid: 31.5 percent.
Example 2.
Adding 1200kg of pure water into a reaction kettle, heating to 80 ℃, starting stirring, and adding 100kg of beta-cyclodextrin into the pure water in batches; stirring and dissolving. 300kg of the benzoic acid in ethanol solution (100 kg of benzoic acid dissolved in 200kg of 95% ethanol in advance) was added dropwise, and the reaction was carried out for 2 hours while maintaining the temperature. Then the reaction solution was subjected to pressure filtration while it was hot and spray-dried (spray-drying conditions: feed temperature: 145 ℃, feed pump flow rate: 25L/h, discharge temperature: 75 ℃) to obtain 191kg of inclusion or coated benzoic acid powder. Yield: 95.5 percent. Content of benzoic acid: 49.2 percent.
Example 3.
Adding 800kg of pure water into a reaction kettle, heating to 60 ℃, starting stirring, and adding 50kg of hydroxypropyl-beta-cyclodextrin into the pure water in batches; stirring and dissolving. 37.5kg of benzoic acid in ethanol (37.5 kg of benzoic acid was dissolved in 75kg of 95% ethanol in advance) was added dropwise, and the mixture was allowed to react for 2 hours under heat. Then, the reaction solution was subjected to pressure filtration while it was hot and spray-dried (spray-drying conditions: feed temperature: 150 ℃, feed pump flow rate: 25L/h, discharge temperature: 80 ℃) to obtain 84kg of inclusion or coated benzoic acid powder. Yield: 96 percent. Content of benzoic acid: 40.5 percent.
Claims (6)
1. An inclusion or coating benzoic acid green preparation process is characterized in that: the feed-grade benzoic acid and cyclodextrin aqueous solution are included to form inclusion or coating benzoic acid solution, and then the inclusion or coating benzoic acid is prepared by spray drying.
2. The green process for the preparation of inclusion or coating benzoic acid according to claim 1, characterized in that: the method comprises the following steps:
(1) adding 5-30 parts of pure water into a reaction kettle, heating to 40-100 ℃, starting stirring, adding 1-5 parts of cyclodextrin into the pure water in batches, and stirring and dissolving uniformly for later use;
(2) dropwise adding 0.1-2 parts of benzoic acid ethanol solution (benzoic acid: 95% ethanol mass ratio =1: 2-4) into the reaction system in the step (1), and after the dropwise adding is finished, carrying out heat preservation reaction for 1-4 hours;
(3) and (3) carrying out pressure filtration on the reaction liquid in the step (2) while the reaction liquid is hot, and then carrying out spray drying to obtain inclusion or coated benzoic acid powder.
3. The green process for the preparation of inclusion or coating benzoic acid according to claim 2, characterized in that: in the step (1), 5-30 parts of pure water is heated at a temperature: 40-100 ℃, cyclodextrin content: 1-5 parts; preferably: pure water amount: 10-20 parts of, heating temperature: 60-80 ℃, cyclodextrin content: 1-2 parts.
4. The green process for the preparation of inclusion or coating benzoic acid according to claim 2, characterized in that: in the step (1), the cyclodextrin is one or more of alpha-cyclodextrin, beta-cyclodextrin, gamma-cyclodextrin, hydroxypropyl-beta-cyclodextrin, methyl-beta-cyclodextrin and sulfobutyl-beta-cyclodextrin.
5. The green process for the preparation of inclusion or coating benzoic acid according to claim 2, characterized in that: in the step (2), 0.1-2 parts of benzoic acid ethanol solution, the mass ratio of benzoic acid to 95% ethanol =1: 2-4, and the reaction time is kept for 1-4 hours; preferably, the following components: ethanol solution of benzoic acid: 0.5-1 part, the mass ratio of benzoic acid to 95% ethanol =1: 2, the heat preservation temperature: and (3) keeping the temperature at 60-80 ℃, and reacting for a time: 2-3 hours.
6. The green process for the preparation of inclusion or coating benzoic acid according to claim 2, characterized in that: in the step (3), the spray drying is to rapidly dry the inclusion or coating benzoic acid solution, and the spray drying conditions are as follows: feeding temperature: 100-200 ℃, flow rate of a feed pump: 5-50L/h, discharge temperature: 50-100 ℃; preferably: feeding temperature: 120-150 ℃, flow rate of a feed pump: 20-30L/h, discharge temperature: 70-80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210213791.0A CN114568588A (en) | 2022-03-05 | 2022-03-05 | Inclusion or coated benzoic acid for feed and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210213791.0A CN114568588A (en) | 2022-03-05 | 2022-03-05 | Inclusion or coated benzoic acid for feed and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN114568588A true CN114568588A (en) | 2022-06-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210213791.0A Withdrawn CN114568588A (en) | 2022-03-05 | 2022-03-05 | Inclusion or coated benzoic acid for feed and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115299553A (en) * | 2022-08-17 | 2022-11-08 | 开封金万德福生物科技有限公司 | Fresh-keeping antidote for feed, production process and use method |
-
2022
- 2022-03-05 CN CN202210213791.0A patent/CN114568588A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115299553A (en) * | 2022-08-17 | 2022-11-08 | 开封金万德福生物科技有限公司 | Fresh-keeping antidote for feed, production process and use method |
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Application publication date: 20220603 |
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