CN112409161A - Preparation method of high-purity feed additive calcium propionate - Google Patents
Preparation method of high-purity feed additive calcium propionate Download PDFInfo
- Publication number
- CN112409161A CN112409161A CN202011318783.XA CN202011318783A CN112409161A CN 112409161 A CN112409161 A CN 112409161A CN 202011318783 A CN202011318783 A CN 202011318783A CN 112409161 A CN112409161 A CN 112409161A
- Authority
- CN
- China
- Prior art keywords
- calcium propionate
- eggshells
- feed additive
- additive calcium
- preparing
- 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.)
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- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 title claims abstract description 26
- 235000010331 calcium propionate Nutrition 0.000 title claims abstract description 26
- 239000004330 calcium propionate Substances 0.000 title claims abstract description 26
- 239000003674 animal food additive Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 210000003278 egg shell Anatomy 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 29
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 16
- 102000002322 Egg Proteins Human genes 0.000 claims abstract description 12
- 108010000912 Egg Proteins Proteins 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 235000019260 propionic acid Nutrition 0.000 claims abstract description 11
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims abstract description 11
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 4
- 239000008399 tap water Substances 0.000 claims abstract description 4
- 235000020679 tap water Nutrition 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000007873 sieving Methods 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000011257 shell material Substances 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- GYPZFDNQZCSGND-UHFFFAOYSA-N propanoic acid;hydrate Chemical compound O.CCC(O)=O GYPZFDNQZCSGND-UHFFFAOYSA-N 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 210000000998 shell membrane Anatomy 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 abstract description 4
- 230000000996 additive effect Effects 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 235000019738 Limestone Nutrition 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- 235000012255 calcium oxide Nutrition 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000004571 lime 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a preparation method of high-purity feed additive calcium propionate, which relates to the field of preparation methods of additive calcium propionate, and the technical scheme is as follows: comprises the following steps of reaction at normal temperature and normal pressure: weighing a proper amount of egg shell powder, putting the egg shell powder into a beaker, adding tap water according to a specified solid-to-liquid ratio, stirring the shell powder solution at a constant speed, slowly adding propionic acid, adding calcium hydroxide powder after the reaction is finished, adjusting the pH of a reaction system, and simplifying the process, reducing the cost and protecting the environment in the process of preparing the additive calcium propionate.
Description
Technical Field
The invention relates to the field of preparation methods of additive calcium propionate, and more particularly relates to a preparation method of high-purity feed additive calcium propionate.
Background
The preparation method of the calcium propionate at present comprises an indirect method and a direct method, wherein in the indirect method process, mainly limestone Sichuan and eggshell rings are used as raw materials, calcined at high temperature to prepare quicklime CaO, then a certain amount of water is added into the CaO to prepare lime milk, a propionic acid solution is slowly added under continuous stirring, the stirring reaction is continued until the solution is clarified to obtain a calcium propionate solution, the filtrate is heated and concentrated to be viscous after being filtered, and the filtrate is dried for 4 hours at 140 ℃ to obtain a white crystalline anhydrous calcium propionate product; the direct method is to directly react propionic acid with industrial calcium carbonate to prepare calcium propionate.
However, among the two methods, the indirect method adopts a high-temperature calcination process, which has high energy consumption and high cost, and generates a large amount of C02 and dust pollution in the calcination process, and the direct method using industrial calcium carbonate as a raw material requires heating in the reaction process, so that the process is complex and the cost is high.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity feed additive calcium propionate, which simplifies the process, reduces the cost and protects the environment in the process of preparing the additive calcium propionate.
The technical purpose of the invention is realized by the following technical scheme: a preparation method of high-purity feed additive calcium propionate comprises the following steps: the method comprises the following steps: (1) pretreatment: soaking the collected eggshells in alkali liquor for 24 hours, and then washing the eggshells clean with clear water to remove attachments and impurities on the surfaces of the eggshells;
(2) shell-membrane separation: adding a separating agent into the eggshells, stirring, standing, pouring out the upper solution, performing suction filtration and recovery on the upper solution, and adding the recovered filtrate into the precipitate;
(3) crushing and sieving: crushing eggshells by a crusher, sieving to ensure that the fineness reaches 100 meshes, crushing the shell materials which do not pass through the crusher again, sieving until all the shell materials pass through the crusher, and bagging for later use;
(4) reaction at normal temperature and normal pressure: weighing a proper amount of eggshell powder, putting the eggshell powder into a beaker, adding tap water, stirring the eggshell powder solution at a constant speed and a liquid-solid ratio of 12:1, slowly adding propionic acid, adding calcium hydroxide powder after the reaction is finished, and adjusting the pH value of the reaction system to 7-8;
(5) and (3) suction filtration: carrying out suction filtration on the materials which are completely reacted, wherein filter residues can be reused, and the pH value of the filtrate is adjusted to 7-8 by propionic acid;
(6) and (3) drying: and pouring the concentrated solution into a tray, and placing the tray in an oven to be dried to obtain the product.
Preferably, the step (5) specifically comprises: adjusting pH of the filtrate with propionic acid, and heating and concentrating the filtrate.
Preferably, the reaction conditions in step (6) are: drying at 130 deg.C for 3-4 hr to obtain the final product.
Preferably, after the step (1) is completed, the cleaned eggshells are put into a drying oven for drying, and after the eggshells are dried for 2 hours at 120 ℃, the eggshells are taken out.
Preferably, several activated carbons are added in said step (1).
Preferably, the separating agent is 2% propionic acid water solution, the stirring time is 5min, and the standing time is 30 min.
Preferably, step (4) involves the chemical reaction equation: CaC03+2CH3CH2COOH=Ca[CH3CH2COO]2+H20+C02。
In conclusion, the invention achieves the following beneficial effects: the method for preparing calcium propionate simplifies the process, reduces the cost and protects the environment, and the eggshells which are regarded as wastes are selected as raw materials to prepare the calcium propionate, so that the pollution of discarding the eggshells can be relieved and eliminated, the chemical pollution of sulfur, arsenic and the like brought by raw coal in the calcining process by limestone can be avoided, and the environment is protected.
Detailed Description
The following examples further illustrate the invention in detail.
Examples
A preparation method of high-purity feed additive calcium propionate comprises the following steps: the method comprises the following steps: (1) pretreatment: soaking the collected eggshells in alkali liquor for 24 hours, and then washing the eggshells clean with clear water to remove attachments and impurities on the surfaces of the eggshells;
(2) shell-membrane separation: adding a separating agent into the eggshells, stirring, standing, pouring out the upper solution, performing suction filtration and recovery on the upper solution, and adding the recovered filtrate into the precipitate;
(3) crushing and sieving: crushing eggshells by a crusher, sieving to ensure that the fineness reaches 100 meshes, crushing the shell materials which do not pass through the crusher again, sieving until all the shell materials pass through the crusher, and bagging for later use;
(4) reaction at normal temperature and normal pressure: weighing a proper amount of eggshell powder, putting the eggshell powder into a beaker, adding tap water, stirring the eggshell powder solution at a constant speed and a liquid-solid ratio of 12:1, slowly adding propionic acid, adding calcium hydroxide powder after the reaction is finished, and adjusting the pH value of the reaction system to 7-8;
(5) and (3) suction filtration: carrying out suction filtration on the materials which are completely reacted, wherein filter residues can be reused, and the pH value of the filtrate is adjusted to 7-8 by propionic acid;
(6) and (3) drying: and pouring the concentrated solution into a tray, and placing the tray in an oven to be dried to obtain the product.
Wherein the separating agent is 2% propionic acid water solution, the stirring time is 5min, the standing time is 30min, and the chemical reaction equation related to the step (4) is as follows: CaC03+2CH3CH2COOH=Ca[CH3CH2COO]2+H20+C02。
In addition, the step (5) specifically includes: adjusting pH of the filtrate with propionic acid, and heating and concentrating the filtrate.
The reaction conditions in step (6) are: drying at 130 deg.C for 3-4 hr to obtain the final product.
And (2) after the step (1) is finished, putting the cleaned eggshells into a drying oven for drying, and taking out the eggshells after drying for 2 hours at 120 ℃.
A plurality of activated carbons are added in the step (1), the effect of adsorbing the eggshells is good, and time is saved.
The method for preparing calcium propionate simplifies the process, reduces the cost and protects the environment, and the eggshells which are regarded as wastes are selected as raw materials to prepare the calcium propionate, so that the pollution of discarding the eggshells can be relieved and eliminated, the chemical pollution of sulfur, arsenic and the like brought by raw coal in the calcining process by limestone can be avoided, and the environment is protected.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (7)
1. A preparation method of high-purity feed additive calcium propionate is characterized by comprising the following steps: (1) pretreatment: soaking the collected eggshells in alkali liquor for 24 hours, and then washing the eggshells clean with clear water to remove attachments and impurities on the surfaces of the eggshells;
(2) shell-membrane separation: adding a separating agent into the eggshells, stirring, standing, pouring out the upper solution, performing suction filtration and recovery on the upper solution, and adding the recovered filtrate into the precipitate;
(3) crushing and sieving: crushing eggshells by a crusher, sieving to ensure that the fineness reaches 100 meshes, crushing the shell materials which do not pass through the crusher again, sieving until all the shell materials pass through the crusher, and bagging for later use;
(4) reaction at normal temperature and normal pressure: weighing a proper amount of eggshell powder, putting the eggshell powder into a beaker, adding tap water, stirring the eggshell powder solution at a constant speed and a liquid-solid ratio of 12:1, slowly adding propionic acid, adding calcium hydroxide powder after the reaction is finished, and adjusting the pH value of the reaction system to 7-8;
(5) and (3) suction filtration: carrying out suction filtration on the materials which are completely reacted, wherein filter residues can be reused, and the pH value of the filtrate is adjusted to 7-8 by propionic acid;
(6) and (3) drying: and pouring the concentrated solution into a tray, and placing the tray in an oven to be dried to obtain the product.
2. The method for preparing the high-purity feed additive calcium propionate as claimed in claim 1, which is characterized in that: the step (5) specifically comprises: adjusting pH of the filtrate with propionic acid, and heating and concentrating the filtrate.
3. The method for preparing the high-purity feed additive calcium propionate as claimed in claim 1, which is characterized in that: the reaction conditions in the step (6) are as follows: drying at 130 deg.C for 3-4 hr to obtain the final product.
4. The method for preparing the high-purity feed additive calcium propionate as claimed in claim 1, which is characterized in that: and (2) after the step (1) is finished, putting the cleaned eggshells into a drying oven for drying, and taking out the eggshells after drying for 2 hours at 120 ℃.
5. The method for preparing the high-purity feed additive calcium propionate as claimed in claim 1, which is characterized in that: adding a plurality of activated carbons in the step (1).
6. The method for preparing the high-purity feed additive calcium propionate as claimed in claim 1, which is characterized in that: the separating agent is 2% propionic acid water solution, and has stirring time of 5min and standing time of 30 min.
7. The method for preparing the high-purity feed additive calcium propionate as claimed in claim 1, which is characterized in that: the chemical reaction equation involved in step (4) is: CaC03+2CH3CH2COOH=Ca[CH3CH2COO]2+H20+C02。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011318783.XA CN112409161A (en) | 2020-11-23 | 2020-11-23 | Preparation method of high-purity feed additive calcium propionate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011318783.XA CN112409161A (en) | 2020-11-23 | 2020-11-23 | Preparation method of high-purity feed additive calcium propionate |
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| Publication Number | Publication Date |
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| CN112409161A true CN112409161A (en) | 2021-02-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202011318783.XA Pending CN112409161A (en) | 2020-11-23 | 2020-11-23 | Preparation method of high-purity feed additive calcium propionate |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4700000A (en) * | 1982-04-28 | 1987-10-13 | Basf Aktiengesellschaft | Preparation of calcium propionate |
| CN1517329A (en) * | 2003-01-16 | 2004-08-04 | 张小燕 | Method of preparing calcium propionate using egg shell |
| CN1927803A (en) * | 2006-09-13 | 2007-03-14 | 陕西今日生物化工科技发展有限责任公司 | Method of preparing calcium propionate and calcium lactate with oyster shell as calcium source |
| CN102675082A (en) * | 2012-04-27 | 2012-09-19 | 华中农业大学 | Preparation method of calcium propionate by egg shell |
| CN102690191A (en) * | 2012-06-11 | 2012-09-26 | 广西工学院 | Method for producing calcium lactate by taking duck egg shell as raw material |
| CN103772183A (en) * | 2012-10-28 | 2014-05-07 | 青岛嘉能节能环保技术有限公司 | Method for preparing lime acetate by using eggshell |
| CN104262132A (en) * | 2014-08-27 | 2015-01-07 | 陕西盛迈石油有限公司 | Method for preparing calcium propionate from eggshell |
-
2020
- 2020-11-23 CN CN202011318783.XA patent/CN112409161A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4700000A (en) * | 1982-04-28 | 1987-10-13 | Basf Aktiengesellschaft | Preparation of calcium propionate |
| CN1517329A (en) * | 2003-01-16 | 2004-08-04 | 张小燕 | Method of preparing calcium propionate using egg shell |
| CN1927803A (en) * | 2006-09-13 | 2007-03-14 | 陕西今日生物化工科技发展有限责任公司 | Method of preparing calcium propionate and calcium lactate with oyster shell as calcium source |
| CN102675082A (en) * | 2012-04-27 | 2012-09-19 | 华中农业大学 | Preparation method of calcium propionate by egg shell |
| CN102690191A (en) * | 2012-06-11 | 2012-09-26 | 广西工学院 | Method for producing calcium lactate by taking duck egg shell as raw material |
| CN103772183A (en) * | 2012-10-28 | 2014-05-07 | 青岛嘉能节能环保技术有限公司 | Method for preparing lime acetate by using eggshell |
| CN104262132A (en) * | 2014-08-27 | 2015-01-07 | 陕西盛迈石油有限公司 | Method for preparing calcium propionate from eggshell |
Non-Patent Citations (3)
| Title |
|---|
| 姜小萍等: "曲面响应法探讨牡蛎壳制备丙酸钙的工艺流程", vol. 37, no. 2, pages 93 - 97 * |
| 徐敏等: "利用蛋壳制备丙酸钙的一种新方法的研究", no. 5, pages 11 - 14 * |
| 陈亚主编: "《现代实用电镀技术》", 国防工业出版社, pages: 554 * |
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Application publication date: 20210226 |
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