WO2018094753A1 - Method for preparing magnesium citrate - Google Patents
Method for preparing magnesium citrate Download PDFInfo
- Publication number
- WO2018094753A1 WO2018094753A1 PCT/CN2016/108189 CN2016108189W WO2018094753A1 WO 2018094753 A1 WO2018094753 A1 WO 2018094753A1 CN 2016108189 W CN2016108189 W CN 2016108189W WO 2018094753 A1 WO2018094753 A1 WO 2018094753A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- citric acid
- magnesium citrate
- magnesium
- citrate
- solution
- Prior art date
Links
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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C59/00—Compounds having carboxyl groups bound to acyclic carbon atoms and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups
- C07C59/235—Saturated compounds containing more than one carboxyl group
- C07C59/245—Saturated compounds containing more than one carboxyl group containing hydroxy or O-metal groups
- C07C59/265—Citric acid
Definitions
- the invention belongs to the field of food and medicine, and particularly relates to a preparation method of magnesium citrate.
- Magnesium citrate is mainly used for pharmaceutical raw materials or food additives, but the current general production method cannot obtain powdered magnesium citrate. .
- the object of the present invention is to solve the deficiencies of the prior art and to provide a method for preparing magnesium citrate.
- a method for preparing magnesium citrate comprising the following steps:
- centrifugal dehydration the prepared magnesium citrate is poured into a mixer and stirred for 48-57 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
- the edible citric acid is added with water to prepare a 46% concentration of citric acid water. Solution.
- the concentration of the copper citrate solution is controlled at Baume d: 1.36.
- the invention has the advantages that the invention adopts edible citric acid, magnesium carbonate or magnesium oxide to carry out the reaction, and the finished product is obtained by material concentration, centrifugal dehydration and drying, without using a catalyst, the process is simple, the energy consumption is low, no pollution, and the cost is low.
- a method for preparing magnesium citrate comprises the following steps:
- centrifugal dehydration the prepared magnesium citrate is poured into a mixer and stirred for 48 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
- a method for preparing magnesium citrate comprises the following steps:
- centrifugal dehydration the prepared magnesium citrate is poured into a mixer and stirred for 57 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
- a method for preparing magnesium citrate comprises the following steps:
- centrifugal dehydration the prepared magnesium citrate is poured into a mixer and stirred for 53 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Disclosed is a method for preparing magnesium citrate, comprising the following steps: raw material preparation – preparation of an aqueous citric acid solution – neutralization reaction – material concentration – centrifugal dehydration – drying. The present invention prepares a finished product by means of reaction of edible citric acid and magnesium carbonate or magnesium oxide, and then material concentration, centrifugal dehydration and drying, without using a catalyst, and therefore has a simple process, low energy consumption, no pollution, and low costs.
Description
本发明属于食品医药领域，具体涉及一种柠檬酸镁的制备方法。The invention belongs to the field of food and medicine, and particularly relates to a preparation method of magnesium citrate.
目前，在国内尚未有详细资料介绍生产柠檬酸镁的方法，更未见有公开的专利，柠檬酸镁主要用于医药原料或食品添加剂，而目前一般的生产方法无法得到粉末状的柠檬酸镁。At present, there is no detailed information on the method of producing magnesium citrate in China, and there is no published patent. Magnesium citrate is mainly used for pharmaceutical raw materials or food additives, but the current general production method cannot obtain powdered magnesium citrate. .
发明内容Summary of the invention
发明目的：本发明的目的是为了解决现有技术的不足，提供一种柠檬酸镁的制备方法。OBJECT OF THE INVENTION: The object of the present invention is to solve the deficiencies of the prior art and to provide a method for preparing magnesium citrate.
技术方案：一种柠檬酸镁的制备方法，包括如下步骤：Technical Solution: A method for preparing magnesium citrate, comprising the following steps:
(1)原料准备：采用食用柠檬酸、碳酸镁或氧化镁为原料；(1) Preparation of raw materials: using edible citric acid, magnesium carbonate or magnesium oxide as raw materials;
(2)配制柠檬酸水溶液：将食用柠檬酸加水配制成43-49％浓度的柠檬酸水溶液；(2) preparing a citric acid aqueous solution: adding edible citric acid to water to prepare a 43-49% concentration aqueous citric acid solution;
(3)中和反应：将上述配制好的柠檬酸水溶液中缓慢加入碳酸镁或氧化镁进行中和反应生成柠檬酸镁控制流量，其中搅拌速度为58-75r/min；(3) Neutralization reaction: the above prepared aqueous citric acid solution is slowly added to the magnesium carbonate or magnesium oxide for neutralization reaction to form a controlled flow rate of magnesium citrate, wherein the stirring speed is 58-75r / min;
(4)物料浓缩：利用反应的中和热，进行再加热使物料浓缩，加热温度为78℃-86℃，柠檬酸镁溶液浓度控制在波美度d：1.35-1.38之间；(4) Material concentration: using the neutralization heat of the reaction, reheating to concentrate the material, the heating temperature is 78 ° C - 86 ° C, the concentration of magnesium citrate solution is controlled between Baume d: 1.35-1.38;
(5)离心脱水：将制备出的柠檬酸镁倒入搅拌机中搅拌48-57min，再放入离心脱水机中进行离心脱水；(5) centrifugal dehydration: the prepared magnesium citrate is poured into a mixer and stirred for 48-57 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
(6)烘干：将脱水后的柠檬酸镁放入78℃-88℃的干燥箱内干燥，得到柠檬酸镁。(6) Drying: The dehydrated magnesium citrate is dried in a drying oven at 78 ° C - 88 ° C to obtain magnesium citrate.
作为优化：所述步骤(2)中，食用柠檬酸加水配制成46％浓度的柠檬酸水
溶液。As an optimization: in the step (2), the edible citric acid is added with water to prepare a 46% concentration of citric acid water.
Solution.
作为优化：所述步骤(4)中，柠檬酸铜溶液浓度控制在波美度d：1.36。As optimization: in the step (4), the concentration of the copper citrate solution is controlled at Baume d: 1.36.
有益效果：本发明采用食用柠檬酸、碳酸镁或氧化镁进行反应，通过物料浓缩、离心脱水、烘干后制得成品，不使用催化剂，工艺简单，耗能低，无污染，成本低。The invention has the advantages that the invention adopts edible citric acid, magnesium carbonate or magnesium oxide to carry out the reaction, and the finished product is obtained by material concentration, centrifugal dehydration and drying, without using a catalyst, the process is simple, the energy consumption is low, no pollution, and the cost is low.
下面结合具体实施例对本发明进行详细阐述。The invention is described in detail below in conjunction with specific embodiments.
具体实施例一：Embodiment 1
一种柠檬酸镁的制备方法，包括如下步骤：A method for preparing magnesium citrate comprises the following steps:
(1)原料准备：采用食用柠檬酸、碳酸镁或氧化镁为原料；(1) Preparation of raw materials: using edible citric acid, magnesium carbonate or magnesium oxide as raw materials;
(2)配制柠檬酸水溶液：将食用柠檬酸加水配制成43％浓度的柠檬酸水溶液；(2) preparing an aqueous solution of citric acid: adding edible citric acid to water to prepare a 43% aqueous solution of citric acid;
(3)中和反应：将上述配制好的柠檬酸水溶液中缓慢加入碳酸镁或氧化镁进行中和反应生成柠檬酸镁控制流量，其中搅拌速度为58r/min；(3) Neutralization reaction: the above prepared aqueous citric acid solution is slowly added to magnesium carbonate or magnesium oxide for neutralization reaction to form a controlled flow rate of magnesium citrate, wherein the stirring speed is 58 r / min;
(4)物料浓缩：利用反应的中和热，进行再加热使物料浓缩，加热温度为78℃，柠檬酸镁溶液浓度控制在波美度d：1.35；(4) Material concentration: using the neutralization heat of the reaction, reheating to concentrate the material, the heating temperature is 78 ° C, the concentration of magnesium citrate solution is controlled at Baume d: 1.35;
(5)离心脱水：将制备出的柠檬酸镁倒入搅拌机中搅拌48min，再放入离心脱水机中进行离心脱水；(5) centrifugal dehydration: the prepared magnesium citrate is poured into a mixer and stirred for 48 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
(6)烘干：将脱水后的柠檬酸镁放入78℃的干燥箱内干燥，得到柠檬酸镁。(6) Drying: The dehydrated magnesium citrate was dried in a drying oven at 78 ° C to obtain magnesium citrate.
具体实施例二：Specific embodiment 2:
一种柠檬酸镁的制备方法，包括如下步骤：A method for preparing magnesium citrate comprises the following steps:
(1)原料准备：采用食用柠檬酸、碳酸镁或氧化镁为原料；(1) Preparation of raw materials: using edible citric acid, magnesium carbonate or magnesium oxide as raw materials;
(2)配制柠檬酸水溶液：将食用柠檬酸加水配制成49％浓度的柠檬酸水溶液；(2) preparing an aqueous solution of citric acid: adding edible citric acid to water to prepare a 49% aqueous solution of citric acid;
(3)中和反应：将上述配制好的柠檬酸水溶液中缓慢加入碳酸镁或氧化镁进行
中和反应生成柠檬酸镁控制流量，其中搅拌速度为75r/min；(3) Neutralization reaction: slowly adding the above prepared citric acid aqueous solution to magnesium carbonate or magnesium oxide
Neutralization reaction produces magnesium citrate control flow rate, wherein the stirring speed is 75r/min;
(4)物料浓缩：利用反应的中和热，进行再加热使物料浓缩，加热温度为86℃，柠檬酸镁溶液浓度控制在波美度d：1.38；(4) Material concentration: using the neutralization heat of the reaction, reheating to concentrate the material, the heating temperature is 86 ° C, the concentration of magnesium citrate solution is controlled at Baume d: 1.38;
(5)离心脱水：将制备出的柠檬酸镁倒入搅拌机中搅拌57min，再放入离心脱水机中进行离心脱水；(5) centrifugal dehydration: the prepared magnesium citrate is poured into a mixer and stirred for 57 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
(6)烘干：将脱水后的柠檬酸镁放入88℃的干燥箱内干燥，得到柠檬酸镁。(6) Drying: The dehydrated magnesium citrate was dried in a drying oven at 88 ° C to obtain magnesium citrate.
具体实施例三：Specific embodiment 3:
一种柠檬酸镁的制备方法，包括如下步骤：A method for preparing magnesium citrate comprises the following steps:
(1)原料准备：采用食用柠檬酸、碳酸镁或氧化镁为原料；(1) Preparation of raw materials: using edible citric acid, magnesium carbonate or magnesium oxide as raw materials;
(2)配制柠檬酸水溶液：将食用柠檬酸加水配制成46％浓度的柠檬酸水溶液；(2) preparing an aqueous solution of citric acid: adding edible citric acid to water to prepare a 46% aqueous solution of citric acid;
(3)中和反应：将上述配制好的柠檬酸水溶液中缓慢加入碳酸镁或氧化镁进行中和反应生成柠檬酸镁控制流量，其中搅拌速度为68r/min；(3) Neutralization reaction: the above prepared aqueous citric acid solution is slowly added to the magnesium carbonate or magnesium oxide for neutralization reaction to form a controlled flow rate of magnesium citrate, wherein the stirring speed is 68r / min;
(4)物料浓缩：利用反应的中和热，进行再加热使物料浓缩，加热温度为82℃，柠檬酸镁溶液浓度控制在波美度d：1.36；(4) Material concentration: using the neutralization heat of the reaction, reheating to concentrate the material, the heating temperature is 82 ° C, the concentration of magnesium citrate solution is controlled at Baume d: 1.36;
(5)离心脱水：将制备出的柠檬酸镁倒入搅拌机中搅拌53min，再放入离心脱水机中进行离心脱水；(5) centrifugal dehydration: the prepared magnesium citrate is poured into a mixer and stirred for 53 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;
(6)烘干：将脱水后的柠檬酸镁放入84℃的干燥箱内干燥，得到柠檬酸镁。(6) Drying: The dehydrated magnesium citrate was dried in a drying oven at 84 ° C to obtain magnesium citrate.
本发明不局限于上述最佳实施方式，任何人在本发明的启示下都可得出其他各种形式的产品，但不论在其形状或结构上作任何变化，凡是具有与本申请相同或相近似的技术方案，均落在本发明的保护范围之内。
The present invention is not limited to the above-described preferred embodiments, and any other form of product can be derived by anyone of the present invention, but without any change in shape or structure, it is the same as or equivalent to the present application. Approximate technical solutions are all within the scope of the present invention.
Claims (3)
- 一种柠檬酸镁的制备方法，其特征在于：包括如下步骤：A method for preparing magnesium citrate, comprising the steps of:(1)原料准备：采用食用柠檬酸、碳酸镁或氧化镁为原料；(1) Preparation of raw materials: using edible citric acid, magnesium carbonate or magnesium oxide as raw materials;(2)配制柠檬酸水溶液：将食用柠檬酸加水配制成43-49％浓度的柠檬酸水溶液；(2) preparing a citric acid aqueous solution: adding edible citric acid to water to prepare a 43-49% concentration aqueous citric acid solution;(3)中和反应：将上述配制好的柠檬酸水溶液中缓慢加入碳酸镁或氧化镁进行中和反应生成柠檬酸镁控制流量，其中搅拌速度为58-75r/min；(3) Neutralization reaction: the above prepared aqueous citric acid solution is slowly added to the magnesium carbonate or magnesium oxide for neutralization reaction to form a controlled flow rate of magnesium citrate, wherein the stirring speed is 58-75r / min;(4)物料浓缩：利用反应的中和热，进行再加热使物料浓缩，加热温度为78℃-86℃，柠檬酸镁溶液浓度控制在波美度d：1.35-1.38之间；(4) Material concentration: using the neutralization heat of the reaction, reheating to concentrate the material, the heating temperature is 78 ° C - 86 ° C, the concentration of magnesium citrate solution is controlled between Baume d: 1.35-1.38;(5)离心脱水：将制备出的柠檬酸镁倒入搅拌机中搅拌48-57min，再放入离心脱水机中进行离心脱水；(5) centrifugal dehydration: the prepared magnesium citrate is poured into a mixer and stirred for 48-57 minutes, and then placed in a centrifugal dehydrator for centrifugal dehydration;(6)烘干：将脱水后的柠檬酸镁放入78℃-88℃的干燥箱内干燥，得到柠檬酸镁。(6) Drying: The dehydrated magnesium citrate is dried in a drying oven at 78 ° C - 88 ° C to obtain magnesium citrate.
- 根据权利要求1所述的柠檬酸镁的制备方法，其特征在于：所述步骤(2)中，食用柠檬酸加水配制成46％浓度的柠檬酸水溶液。The method for preparing magnesium citrate according to claim 1, wherein in the step (2), the edible citric acid is added with water to prepare a 46% aqueous solution of citric acid.
- 根据权利要求1所述的柠檬酸镁的制备方法，其特征在于：所述步骤(4)中，柠檬酸铜溶液浓度控制在波美度d：1.36。 The method for preparing magnesium citrate according to claim 1, wherein in the step (4), the concentration of the copper citrate solution is controlled at a Baume degree d: 1.36.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611049828.1 | 2016-11-25 | ||
| CN201611049828 | 2016-11-25 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2018094753A1 true WO2018094753A1 (en) | 2018-05-31 |
Family
ID=62196104
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/CN2016/108189 WO2018094753A1 (en) | 2016-11-25 | 2016-12-01 | Method for preparing magnesium citrate |
Country Status (1)
| Country | Link |
|---|---|
| WO (1) | WO2018094753A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111671091A (en) * | 2020-06-19 | 2020-09-18 | 连云港东泰食品配料有限公司 | Production method of magnesium citrate and magnesium oxide composite product |
| RU2748796C1 (en) * | 2020-10-21 | 2021-05-31 | Акционерное общество "Научно-производственное предприятие "Радий" | Method for producing magnesium citrate and its derivatives |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591234A (en) * | 2008-05-26 | 2009-12-02 | 南通市飞宇精细化学品有限公司 | A kind of method of producing magnesium citrate |
| CN102285877A (en) * | 2010-06-17 | 2011-12-21 | 陆生杰 | Method for producing magnesium citrate |
| CN104447272A (en) * | 2014-11-14 | 2015-03-25 | 宁乡新阳化工有限公司 | Production method of magnesium citrate anhydrous |
-
2016
- 2016-12-01 WO PCT/CN2016/108189 patent/WO2018094753A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591234A (en) * | 2008-05-26 | 2009-12-02 | 南通市飞宇精细化学品有限公司 | A kind of method of producing magnesium citrate |
| CN102285877A (en) * | 2010-06-17 | 2011-12-21 | 陆生杰 | Method for producing magnesium citrate |
| CN104447272A (en) * | 2014-11-14 | 2015-03-25 | 宁乡新阳化工有限公司 | Production method of magnesium citrate anhydrous |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111671091A (en) * | 2020-06-19 | 2020-09-18 | 连云港东泰食品配料有限公司 | Production method of magnesium citrate and magnesium oxide composite product |
| CN111671091B (en) * | 2020-06-19 | 2022-02-08 | 连云港东泰食品配料有限公司 | Production method of magnesium citrate and magnesium oxide composite product |
| RU2748796C1 (en) * | 2020-10-21 | 2021-05-31 | Акционерное общество "Научно-производственное предприятие "Радий" | Method for producing magnesium citrate and its derivatives |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103783231B (en) | Production method for jasmine flower flavor type black tea | |
| CN104478704A (en) | Preparation method of anhydrous trisodium citrate | |
| WO2018094753A1 (en) | Method for preparing magnesium citrate | |
| CN103803662B (en) | A kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate | |
| CN103449977B (en) | A kind of production method of pyrogallol | |
| CN105669439B (en) | The method for preparing potassium sorbate using ceramic membrane reactor | |
| WO2018094755A1 (en) | Method for preparing copper citrate | |
| CN103008020A (en) | Production method of strong-acid compound styrene cation exchange resin | |
| WO2018094754A1 (en) | Method for preparing selenium citrate | |
| CN104445221A (en) | New microwave-assisted method for preparing white carbon black from rice hull ash | |
| CN112778148A (en) | Preparation method of EDDHA chelated iron salt | |
| CN104557519A (en) | Production technique of selenium citrate | |
| CN104743645A (en) | Method for producing polyaluminum ferric chloride by using Bayer red mud | |
| CN106673032B (en) | A kind of peracidity low-crystallinity alumina dry glue and preparation method thereof | |
| CN103275338B (en) | A kind of method adopting glutaraldehyde to improve gracilaria agar gel strength | |
| CN105413716A (en) | Post-neutralization preparation method of vanadium catalyst | |
| CN104291367B (en) | A kind of production method of magnesium sulfate monohydrate | |
| CN104529753B (en) | A kind of production technology of citric acid boron | |
| CN103950979B (en) | Simple and effective energy-conservation niobic acid preparation method | |
| CN106187742A (en) | A kind of efficient calcium acetate preparation method | |
| CN104058438A (en) | Preparation method of aluminium fluoride | |
| CN107697951A (en) | A kind of method for preparing chromium sulfate basic using chromium system resin column regenerated liquid | |
| CN102178263A (en) | Method for drying duck egg powder by micro wave | |
| CN107874100A (en) | A kind of preparation method of sophora bud health nutritious noodle | |
| CN204594115U (en) | A kind of baking oven of improvement |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 16922172 Country of ref document: EP Kind code of ref document: A1 |
|
| NENP | Non-entry into the national phase |
Ref country code: DE |
|
| 122 | Ep: pct application non-entry in european phase |
Ref document number: 16922172 Country of ref document: EP Kind code of ref document: A1 |