CN111671091B - Production method of magnesium citrate and magnesium oxide composite product - Google Patents

Production method of magnesium citrate and magnesium oxide composite product Download PDF

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Publication number
CN111671091B
CN111671091B CN202010563121.2A CN202010563121A CN111671091B CN 111671091 B CN111671091 B CN 111671091B CN 202010563121 A CN202010563121 A CN 202010563121A CN 111671091 B CN111671091 B CN 111671091B
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magnesium
magnesium oxide
reaction
citrate
composite product
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CN111671091A (en
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卞其华
杨威
周洺阳
舒峰
纪玉英
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Lianyungang Dongtai Food Ingredients Co ltd
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Lianyungang Dongtai Food Ingredients Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16Inorganic salts, minerals or trace elements
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/02Magnesia
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mycology (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention belongs to the field of inorganic chemical synthesis, and discloses a production method of a magnesium citrate/magnesium oxide composite product. The production method of the magnesium citrate/magnesium oxide composite product comprises the following steps: (1) adding a citric acid monohydrate solution with the mass concentration of 10-20% into a reaction kettle, heating to 50-60 ℃, adding magnesium oxide slurry with the mass concentration of 10-20% into the reaction kettle, and controlling the pH value at the end point of the reaction to be 6-8; (2) and (2) after the reaction in the step (1) is finished, concentrating the reaction solution until crystals are separated out, continuously adding magnesium oxide until the concentration of the crystals is 40-60%, carrying out solid-liquid separation, and drying for 6-8 hours to obtain the magnesium citrate/magnesium oxide composite product. The magnesium content of the magnesium citrate/magnesium oxide composite product obtained by the method can reach 30-35%, and the problems that the magnesium citrate product is single in specification and the magnesium content is difficult to improve are solved.

Description

Production method of magnesium citrate and magnesium oxide composite product
Technical Field
The invention relates to the field of inorganic chemical synthesis, in particular to a production method of a magnesium citrate/magnesium oxide composite product.
Background
Magnesium citrate, also known as citric acid or magnesium salt, is a white or yellowish powder formed from magnesium carbonate and citric acid, non-toxic, non-corrosive. Magnesium citrate is a chemical preparation with medicinal value, generally has the magnesium content as high as eleven percent, is often used as a health-care nutritional supplement because the magnesium component is easily absorbed by a human body, and is an important magnesium nutritional supplement source.
The most common medical use of magnesium citrate is as a normal saline laxative. Magnesium citrate is provided to the patient prior to any surgery to facilitate emptying of the intestine. This is because magnesium citrate tends to absorb tissue water, and can absorb a large amount of water and discharge it to the outside of the body after being injected into the intestinal tract. In fact, it can also treat constipation and colon cancer, or diseases associated with rectal cancer. In addition, magnesium citrate has the effect of preventing kidney stones.
When the magnesium citrate is used for medical application, the quality requirement on the magnesium citrate is high. Therefore, much attention has been paid to the prior art to reduce the impurity content of magnesium citrate products. For example, chinese patent application CN106854145 provides a method for producing magnesium citrate crystals, and magnesium citrate crystals produced by the method, aiming at overcoming the defects that the prior art method for producing magnesium citrate crystals is easy to cause reactant inclusion and excessive amount, so as to result in the magnesium citrate crystals doped with reactants, and the content of the magnesium citrate crystals is low. For another example, chinese patent applications CN102285877 and CN101591234 provide a method for producing magnesium citrate to reduce lead heavy metals brought in during the production of magnesium citrate.
Magnesium citrate is an important source of magnesium nutrition supplement, and is often used as a health care nutrition supplement because of its high magnesium content and its magnesium component is easily absorbed by human body. However, although the magnesium content of magnesium citrate is high, the magnesium content is only eleven percent, the current production technology only remains in the improvement of the magnesium citrate content, and no synthesis method for magnesium citrate products with high magnesium content is reported.
Disclosure of Invention
The invention aims to overcome the defects of the background art and provides a production method of a magnesium citrate/magnesium oxide composite product, the magnesium content of the obtained magnesium citrate/magnesium oxide composite product can reach 30-35%, and the problems that the specification of the magnesium citrate product is single and the magnesium content is difficult to improve are solved.
In order to achieve the purpose of the invention, the method for producing the magnesium citrate/magnesium oxide composite product comprises the following steps:
(1) adding a citric acid monohydrate solution with the mass concentration of 10-20% into a reaction kettle, heating to 50-60 ℃, adding magnesium oxide slurry with the mass concentration of 10-20% into the reaction kettle, and controlling the pH value at the end point of the reaction to be 6-8;
(2) and (2) after the reaction in the step (1) is finished, concentrating the reaction solution until crystals are separated out, continuously adding magnesium oxide until the concentration of the crystals is 40-60%, carrying out solid-liquid separation, and drying for 6-8 hours to obtain the magnesium citrate/magnesium oxide composite product.
Further, the citric acid monohydrate, magnesium oxide are food grade.
Further, heating to 50-60 ℃ in the step (1) is carried out by heating with steam through a jacket.
In the invention, as the magnesium oxide is added to release heat, the citric acid monohydrate solution is added into the reaction kettle and then heated to 50-60 ℃, and then the magnesium oxide is added.
Further, in the step (1), the reaction temperature is controlled to be 60-80 ℃ for 2-4 hours.
Furthermore, the volume ratio of the citric acid monohydrate solution to the magnesium oxide slurry in the step (1) is 50: 6-20.
Further, the drying in the step (2) is carried out by controlling the temperature to be 120-150 ℃.
Further, the high magnesium content means that the magnesium content of the obtained magnesium citrate/magnesium oxide composite product reaches more than 30%, and further means that the magnesium content of the obtained magnesium citrate/magnesium oxide composite product reaches 30-35%.
Compared with the prior art, the magnesium content of the magnesium citrate/magnesium oxide composite product prepared by the method can reach 30-35%, the preparation method is different from simple physical mixing and compounding, the product is formed by mixed crystals of magnesium citrate and magnesium oxide, the crystallinity is good, the production method of the magnesium citrate crystal product with high magnesium content is developed, and the application range of the magnesium citrate product is expanded.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", etc. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
500L of food-grade citric acid monohydrate solution with the mass concentration of 10% is added into a 1000L reaction kettle, steam is introduced into a jacket to heat the mixture to 50 ℃, 60L of food-grade magnesium oxide slurry with the mass concentration of 15% is added into the reaction kettle, the reaction temperature is controlled to be 60 ℃, the reaction time is 4 hours, and the pH value at the end of the reaction is 7.0.
After the reaction is finished, concentrating the reaction liquid until crystals are separated out, continuously adding food-grade magnesium oxide until the concentration of the crystals is 45%, after solid-liquid separation, controlling the temperature to be 150 ℃ and drying for about 6 hours to obtain a magnesium citrate/magnesium oxide composite product, wherein the magnesium content of the product is 31.5%.
Example 2
Adding 500L of food-grade citric acid monohydrate solution with the mass concentration of 20% into a 1000L reaction kettle, introducing steam into a jacket to heat the mixture to 60 ℃, adding 200L of food-grade magnesium oxide slurry with the mass concentration of 10% into the reaction kettle, controlling the reaction temperature to be 80 ℃, reacting for 2 hours, and controlling the pH value at the end point of the reaction to be 6.5.
After the reaction is finished, concentrating the reaction liquid until crystals are separated out, continuously adding food-grade magnesium oxide until the concentration of the crystals is 50%, after solid-liquid separation, controlling the temperature to be 120 ℃ and drying for about 8 hours to obtain a magnesium citrate product with high magnesium content, wherein the magnesium content of the product reaches 33%.
Example 3
500L of food-grade citric acid monohydrate solution with the mass concentration of 15 percent is added into a 1000L reaction kettle, steam is introduced into a jacket to heat the mixture to 60 ℃, 150L of food-grade magnesium oxide slurry with the mass concentration of 10 percent is added into the reaction kettle, the reaction temperature is controlled to be 75 ℃, the reaction time is 3 hours, and the pH value at the end of the reaction is 8.0.
After the reaction is finished, concentrating the reaction liquid until crystals are separated out, continuously adding food-grade magnesium oxide until the concentration of the crystals is 60%, and after solid-liquid separation, drying at 125 ℃ for about 8 hours to obtain a magnesium citrate product with high magnesium content, wherein the magnesium content of the product reaches 34.5%.
Comparative example 1
500L of food-grade citric acid monohydrate solution with the mass concentration of 10% is added into a 1000L reaction kettle, steam is introduced into a jacket to heat the mixture to 50 ℃, 60L of food-grade magnesium oxide slurry with the mass concentration of 15% is added into the reaction kettle, the reaction temperature is controlled to be 60 ℃, the reaction time is 4 hours, and the pH value at the end of the reaction is 7.0.
After the reaction is finished, concentrating the reaction liquid until crystals are separated out, continuously adding food-grade magnesium oxide until the concentration of the crystals is 70%, after solid-liquid separation, controlling the temperature to be 150 ℃ and drying for about 6 hours to obtain a magnesium citrate/magnesium oxide composite product, wherein the magnesium content of the product is 21.1%.
Comparative example 2
500L of food-grade citric acid monohydrate solution with the mass concentration of 10% is added into a 1000L reaction kettle, steam is introduced into a jacket to heat the mixture to 50 ℃, 60L of food-grade magnesium oxide slurry with the mass concentration of 15% is added into the reaction kettle, the reaction temperature is controlled to be 60 ℃, the reaction time is 4 hours, and the pH value at the end of the reaction is 7.0.
After the reaction is finished, concentrating the reaction liquid until crystals are separated out, continuously adding food-grade magnesium oxide until the concentration of the crystals is 30%, after solid-liquid separation, controlling the temperature to be 150 ℃ and drying for about 6 hours to obtain a magnesium citrate/magnesium oxide composite product, wherein the magnesium content of the product is 16.7%.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.

Claims (3)

1. A method for producing a magnesium citrate and magnesium oxide composite product is characterized by comprising the following steps of:
(1) adding a citric acid monohydrate solution with the mass concentration of 10-20% into a reaction kettle, heating to 50-60 ℃, adding magnesium oxide slurry with the mass concentration of 10-20% into the reaction kettle, and controlling the pH value at the end point of the reaction to be 6-8;
(2) concentrating the reaction solution after the reaction in the step (1) until crystals are separated out, continuously adding magnesium oxide until the concentration of the crystals is 40-60%, carrying out solid-liquid separation, and drying for 6-8 hours to obtain a magnesium citrate and magnesium oxide composite product; controlling the reaction temperature in the step (1) to be 60-80 ℃ for reacting for 2-4 hours;
the volume ratio of the citric acid monohydrate solution to the magnesium oxide slurry in the step (1) is 50: 6-20;
the drying in the step (2) is carried out by controlling the temperature to be 120-150 ℃;
the magnesium content of the magnesium citrate and magnesium oxide composite product is up to 30-35%.
2. The method for producing magnesium citrate magnesium oxide composite product according to claim 1, wherein the citric acid monohydrate and magnesium oxide are food grade.
3. The method for producing magnesium citrate-magnesium oxide composite product according to claim 1, wherein the heating to 50-60 ℃ in step (1) is jacket-steam heating.
CN202010563121.2A 2020-06-19 2020-06-19 Production method of magnesium citrate and magnesium oxide composite product Active CN111671091B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102285877A (en) * 2010-06-17 2011-12-21 陆生杰 Method for producing magnesium citrate
WO2018094753A1 (en) * 2016-11-25 2018-05-31 南通市飞宇精细化学品有限公司 Method for preparing magnesium citrate
EP3338772A1 (en) * 2016-12-22 2018-06-27 Merz Pharma GmbH & Co. KGaA Trimagnesiumdicitrate compositions stabilized by hydroxycarboxylic acids , the production thereof and highly concentrated magnesium compositions

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06228046A (en) * 1993-02-05 1994-08-16 Tomita Seiyaku Kk Production of magnesium hydrogen citrate pentahydrate
CN103880060A (en) * 2014-02-24 2014-06-25 南通励成生物工程有限公司 Method for producing high-purity zinc salt for food or health-care products
CN104447272A (en) * 2014-11-14 2015-03-25 宁乡新阳化工有限公司 Production method of magnesium citrate anhydrous
CN106854155A (en) * 2015-12-08 2017-06-16 中粮生物化学(安徽)股份有限公司 A kind of preparation of magnesium salts of citric acid and preparation method thereof and the magnesium salts containing the citric acid
CN106854145A (en) * 2015-12-08 2017-06-16 中粮生物化学(安徽)股份有限公司 A kind of magnesium citrate crystal and its production method
CN110002991A (en) * 2019-04-09 2019-07-12 宁乡新阳化工有限公司 A kind of production method for mending magnesium raw material magnesium acid citrate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102285877A (en) * 2010-06-17 2011-12-21 陆生杰 Method for producing magnesium citrate
WO2018094753A1 (en) * 2016-11-25 2018-05-31 南通市飞宇精细化学品有限公司 Method for preparing magnesium citrate
EP3338772A1 (en) * 2016-12-22 2018-06-27 Merz Pharma GmbH & Co. KGaA Trimagnesiumdicitrate compositions stabilized by hydroxycarboxylic acids , the production thereof and highly concentrated magnesium compositions

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