CN115626882A - Method for purifying creatine monohydrate - Google Patents
Method for purifying creatine monohydrate Download PDFInfo
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- CN115626882A CN115626882A CN202211326607.XA CN202211326607A CN115626882A CN 115626882 A CN115626882 A CN 115626882A CN 202211326607 A CN202211326607 A CN 202211326607A CN 115626882 A CN115626882 A CN 115626882A
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- creatine monohydrate
- creatine
- monohydrate
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- MEJYXFHCRXAUIL-UHFFFAOYSA-N 2-[carbamimidoyl(methyl)amino]acetic acid;hydrate Chemical compound O.NC(=N)N(C)CC(O)=O MEJYXFHCRXAUIL-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229960004826 creatine monohydrate Drugs 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 46
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 62
- CVSVTCORWBXHQV-UHFFFAOYSA-N creatine Chemical compound NC(=[NH2+])N(C)CC([O-])=O CVSVTCORWBXHQV-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000047 product Substances 0.000 claims abstract description 39
- 238000001914 filtration Methods 0.000 claims abstract description 27
- 229960003624 creatine Drugs 0.000 claims abstract description 23
- 239000006046 creatine Substances 0.000 claims abstract description 23
- 239000000706 filtrate Substances 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000746 purification Methods 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims description 33
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 25
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 22
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 14
- 229940109239 creatinine Drugs 0.000 claims description 9
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 abstract description 20
- 238000001035 drying Methods 0.000 abstract description 8
- 239000012535 impurity Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000012824 chemical production Methods 0.000 abstract description 2
- 230000007935 neutral effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 210000003205 muscle Anatomy 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- 206010049565 Muscle fatigue Diseases 0.000 description 1
- 108010077895 Sarcosine Proteins 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 235000015872 dietary supplement Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 201000006938 muscular dystrophy Diseases 0.000 description 1
- VILYDVYHBMHOSG-UHFFFAOYSA-M potassium;2-(methylamino)acetate Chemical compound [K+].CNCC([O-])=O VILYDVYHBMHOSG-UHFFFAOYSA-M 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229940048098 sodium sarcosinate Drugs 0.000 description 1
- ZUFONQSOSYEWCN-UHFFFAOYSA-M sodium;2-(methylamino)acetate Chemical compound [Na+].CNCC([O-])=O ZUFONQSOSYEWCN-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C279/00—Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C279/04—Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of guanidine groups bound to acyclic carbon atoms of a carbon skeleton
- C07C279/14—Derivatives of guanidine, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups having nitrogen atoms of guanidine groups bound to acyclic carbon atoms of a carbon skeleton being further substituted by carboxyl groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of chemical production, and particularly discloses a method for purifying creatine monohydrate. The method for purifying the creatine monohydrate provided by the invention uses the creatine monohydrate with low purity as a raw material, firstly adds water into the creatine with low content and stirs the mixture, then uses hydrochloric acid to adjust the pH value to completely dissolve the creatine, then adds active carbon to decolor and remove impurities, and then filters the solution, and adjusts the pH value of the obtained filtrate back to be neutral, thus obtaining creatine monohydrate feed liquid; filtering the feed liquid, and drying a filter cake to obtain a qualified creatine monohydrate product. The method has the advantages of simple process, simple condition requirement, high recovery rate and high product content, can treat unqualified creatine monohydrate materials to obtain purified creatine monohydrate, has high creatine monohydrate content after purification, and can meet various index requirements.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a method for purifying creatine monohydrate.
Background
The creatine monohydrate can inhibit the generation of muscle fatigue factors, relieve fatigue and tension, recover physical fitness, accelerate the synthesis of human body protein, make muscles firmer, enhance the muscle elasticity, reduce cholesterol, blood fat and blood sugar levels, improve the muscular dystrophy of middle-aged and elderly people, and delay aging. Creatine monohydrate is praised as one of the most desirable and effective nutritional supplements, and is high enough to be driven by protein products.
The existing creatine preparation technology is mainly to react cyanamide with an aqueous solution of sodium sarcosinate or potassium sarcosinate to prepare the creatine monohydrate, but in actual production, the prepared creatine monohydrate has low purity and poor product quality, and needs to be purified again to obtain a high-quality creatine monohydrate product. At present, for creatine monohydrate with low content or creatine monohydrate containing a large amount of impurities, an effective purification method is not available, and a high-quality creatine monohydrate product cannot be obtained through purification, so that resource waste is caused. On the other hand, the creatine monohydrate produced at present is mostly used as a food additive, so the requirements on the content of the creatine monohydrate and related physical and chemical indexes are strict, and if the creatine monohydrate has unqualified content or a material partially polluted by external impurities exists in the production process, the creatine monohydrate can only be recovered, but a proper process is lacked for purifying the creatine, so the environmental protection pressure and the production cost are greatly increased.
The invention provides a purification method of low-content creatine monohydrate, aiming at the problems of low content of creatine monohydrate, high impurity content and difficult treatment and utilization, so as to obtain a high-purity creatine monohydrate product.
Disclosure of Invention
The invention mainly solves the technical problem of providing a creatine monohydrate purification method which can obtain a creatine monohydrate product with high purity and is simple and easy to implement.
In order to solve the technical problem, the invention provides a method for purifying creatine monohydrate, which comprises the following steps:
(1) Mixing creatine monohydrate with water, and then adding acid until the creatine monohydrate is completely dissolved to obtain a creatine solution;
(2) Adding activated carbon into the creatine solution for treatment, and filtering to obtain filtrate;
(3) And adjusting the pH of the filtrate to 6-8 with alkali liquor, stirring, and filtering to obtain a filter cake, namely the creatine monohydrate product.
As a preferred embodiment of the present invention, the creatine monohydrate has a purity of 80 to 92%, more preferably the creatine monohydrate has a purity of 80 to 90%.
As a preferred embodiment of the present invention, the creatine monohydrate and water are mixed in a mass ratio of 1: (4-10), and further preferably mixing the components in a mass ratio of 1: (4-6), more preferably mixing in a mass ratio of 1:4, mixing.
In a preferred embodiment of the present invention, in step (1), the acid is hydrochloric acid, preferably the concentration of hydrochloric acid is 28 to 33% by mass, and more preferably the concentration of hydrochloric acid is 30% by mass.
As a preferred embodiment of the present invention, in the step (1), the temperature of the reaction system is controlled to 10 ℃ or lower during the addition of hydrochloric acid.
Preferably, in the step (1), when acid is added until the pH of the reaction system is 1-4, the creatine monohydrate is completely dissolved, and the addition of hydrochloric acid is stopped to obtain a creatine solution.
As a preferred embodiment of the present invention, in the step (2), the temperature of the reaction system is controlled to be 10 ℃ or lower during the treatment of the creatine solution with activated carbon.
Preferably, the addition amount of the activated carbon is 0.1-1.0% of the weight of the creatine monohydrate raw material, and more preferably, the addition amount of the activated carbon is 0.4-0.6% of the weight of the creatine monohydrate raw material.
In a preferred embodiment of the present invention, in the step (3), the alkali solution is ammonia water, preferably, the mass percentage concentration of the ammonia water is 15-25%, and further preferably, the mass percentage concentration of the ammonia water is 20%.
Preferably, the temperature of the reaction system is controlled below 10 ℃ during the addition of the alkali liquor.
Further preferably, the pH of the filtrate is adjusted to 7-8 with an alkali liquor, the addition of the alkali liquor is stopped, and the filtrate is filtered after being stirred.
In a preferred embodiment of the present invention, in the step (3), the temperature of the feed liquid during the filtration is 15 to 20 ℃.
As a preferred embodiment of the present invention, in step (3), the filter cake is dried to obtain a creatine monohydrate product. Wherein the purity of the creatine monohydrate product is more than or equal to 99.0 percent, the content of dicyandiamide is less than or equal to 20ppm, and the content of creatinine is less than or equal to 50ppm.
The invention also provides a creatine monohydrate product obtained by the purification method.
The invention provides a method for purifying creatine monohydrate, which takes creatine monohydrate with low purity as a raw material, wherein the creatine monohydrate with low purity is mainly from creatine monohydrate with insufficient content or high impurity content in the production, and qualified creatine monohydrate products can be obtained through the treatment of the method. Specifically, the low-content creatine monohydrate is added with water and stirred, then hydrochloric acid is used for adjusting the pH value to completely dissolve the creatine, then activated carbon is added for decoloration and impurity removal, then filtration is carried out, the pH value of the obtained filtrate is adjusted back to be neutral, and creatine monohydrate feed liquid is obtained; filtering the feed liquid, and drying a filter cake to obtain a qualified creatine monohydrate product.
The method is an efficient creatine monohydrate purification method, uses less energy, does not use other organic reagents or compounds, is environment-friendly and safe, has low requirement on equipment, short reaction time and simple steps, and the purified product has high purity and high recovery rate. The method has the advantages of simple process, simple condition requirement, high recovery rate and high product content, and can treat unqualified creatine monohydrate materials to obtain purified creatine monohydrate, wherein the content of the purified creatine monohydrate can reach 99.0 percent or even more than 99.5 percent, and meets various index requirements.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments. It will be understood by those skilled in the art that the embodiments described below are merely illustrative of the present invention and should not be construed as limiting the scope of the invention. All other embodiments, such as modifications and substitutions, which can be obtained by one skilled in the art based on the embodiments of the present invention without any inventive step, belong to the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the raw materials, reagents, instruments and the like used are commercially available unless otherwise specified.
The percentages in the following examples and comparative examples are percentages by mass.
Example 1
This embodiment provides a method for purifying creatine monohydrate, comprising the steps of:
(1) Taking 100g of creatine monohydrate with the purity of 90%, stirring and mixing with 400g of pure water, then dropwise adding hydrochloric acid with the mass percentage concentration of 30% into the mixture until the creatine monohydrate is completely dissolved, wherein the pH value of a reaction system is 1.5, stopping dropwise adding the hydrochloric acid to obtain a creatine solution, and controlling the temperature of the reaction system to be below 10 ℃ in the process of dropwise adding the hydrochloric acid;
(2) Adding 0.5g of active carbon into the creatine solution, stirring for 30min, controlling the temperature of a reaction system to be below 10 ℃, and then filtering to obtain filtrate;
(3) And (3) dropwise adding ammonia water with the mass percentage concentration of 20% into the filtrate to adjust the pH value to 7.2, stopping dropwise adding the ammonia water, controlling the temperature of a reaction system to be below 10 ℃ in the dropwise adding process of the ammonia water, then keeping the temperature and stirring for 1h, filtering, wherein the temperature of feed liquid during filtering is 19 ℃, obtaining a filter cake which is a creatine monohydrate wet product, and drying to obtain 80g of creatine monohydrate product.
The purity of the creatine monohydrate product is 99.6 percent, wherein the content of dicyandiamide is less than or equal to 20ppm, and the content of creatinine is less than or equal to 50ppm.
Example 2
This embodiment provides a method for purifying creatine monohydrate, comprising the steps of:
(1) Taking 100g of creatine monohydrate with the purity of 90%, stirring and mixing with 400g of pure water, then dropwise adding hydrochloric acid with the mass percentage concentration of 30% into the mixture until the creatine monohydrate is completely dissolved, wherein the pH value of a reaction system is 1.5, stopping dropwise adding the hydrochloric acid to obtain a creatine solution, and controlling the temperature of the reaction system to be below 10 ℃ in the process of dropwise adding the hydrochloric acid;
(2) Adding 0.6g of active carbon into the creatine solution, stirring for 30min, controlling the temperature of a reaction system to be below 10 ℃, and then filtering to obtain filtrate;
(3) And (3) dropwise adding ammonia water with the mass percentage concentration of 20% into the filtrate to adjust the pH value to 7.4, stopping dropwise adding the ammonia water, controlling the temperature of a reaction system to be below 10 ℃ in the dropwise adding process of the ammonia water, then keeping the temperature and stirring for 1h, filtering, wherein the temperature of feed liquid during filtering is 18 ℃, obtaining a filter cake which is a creatine monohydrate wet product, and drying to obtain the creatine monohydrate product of 81g in total.
The purity of the creatine monohydrate product is 99.7 percent, wherein the content of dicyandiamide is less than or equal to 20ppm, and the content of creatinine is less than or equal to 50ppm.
Example 3
This example provides a method for purifying creatine monohydrate, comprising the steps of:
(1) Taking 100g of creatine monohydrate with the purity of 90%, stirring and mixing with 600g of pure water, then dropwise adding hydrochloric acid with the mass percentage concentration of 30% into the mixture until the creatine monohydrate is completely dissolved, wherein the pH value of a reaction system is 1.5, stopping dropwise adding the hydrochloric acid to obtain a creatine solution, and controlling the temperature of the reaction system to be below 10 ℃ in the hydrochloric acid dropwise adding process;
(2) Adding 0.5g of activated carbon into the creatine solution, stirring for 30min, controlling the temperature of a reaction system below 10 ℃, and then filtering to obtain filtrate;
(3) And (3) dropwise adding ammonia water with the mass percentage concentration of 20% into the filtrate to adjust the pH value to 7.4, stopping dropwise adding the ammonia water, controlling the temperature of a reaction system to be below 10 ℃ in the dropwise adding process of the ammonia water, then keeping the temperature and stirring for 1h, filtering, wherein the temperature of feed liquid during filtering is 19 ℃, obtaining a filter cake which is a creatine monohydrate wet product, and drying to obtain the creatine monohydrate product of 72g in total.
The purity of the creatine monohydrate product is 99.4 percent, wherein the content of dicyandiamide is less than or equal to 20ppm, and the content of creatinine is less than or equal to 50ppm.
Comparative example 1
The present comparative example provides a method for purifying creatine monohydrate, comprising the steps of:
(1) Taking 100g of creatine monohydrate with the purity of 90%, stirring and mixing with 300g of pure water, then dropwise adding hydrochloric acid with the mass percentage concentration of 30% into the mixture until the creatine monohydrate is completely dissolved, wherein the pH value of a reaction system is 1.5, stopping dropwise adding the hydrochloric acid to obtain a creatine solution, and controlling the temperature of the reaction system to be below 10 ℃ in the process of dropwise adding the hydrochloric acid;
(2) Adding 0.5g of active carbon into the creatine solution, stirring for 30min, controlling the temperature of a reaction system to be below 10 ℃, and then filtering to obtain filtrate;
(3) And (2) dropwise adding ammonia water with the mass percentage concentration of 20% into the filtrate to adjust the pH value to 7.4, stopping dropwise adding the ammonia water, controlling the temperature of a reaction system to be below 10 ℃ in the dropwise adding process of the ammonia water, then keeping the temperature and stirring for 1h, filtering, wherein the temperature of feed liquid during filtering is 20 ℃, and obtaining a filter cake, namely a creatine monohydrate wet product, and drying to obtain the creatine monohydrate product of 81g in total.
The purity of the creatine monohydrate product was 95.4% with 100ppm dicyandiamide and 350ppm creatinine.
In comparison, it is found that the decrease of the amount of pure water mixed with the creatine monohydrate raw material directly affects the quality of the creatine monohydrate product obtained by purification, resulting in decreased purity and increased impurity content.
Comparative example 2
The present comparative example provides a method for purifying creatine monohydrate, comprising the steps of:
(1) Taking 100g of creatine monohydrate with the purity of 90%, stirring and mixing with 400g of pure water, then dropwise adding hydrochloric acid with the mass percentage concentration of 30% into the mixture until the creatine monohydrate is completely dissolved, wherein the pH of a reaction system is 1.5, stopping dropwise adding the hydrochloric acid to obtain a creatine solution, and controlling the temperature of the reaction system to be 28-30 ℃ in the process of dropwise adding the hydrochloric acid;
(2) Adding 0.5g of active carbon into the creatine solution, stirring for 30min, controlling the temperature of a reaction system to be below 10 ℃, and then filtering to obtain filtrate;
(3) And (3) dropwise adding ammonia water with the mass percentage concentration of 20% into the filtrate to adjust the pH value to 7.4, stopping dropwise adding the ammonia water, controlling the temperature of a reaction system to be below 10 ℃ in the dropwise adding process of the ammonia water, then keeping the temperature and stirring for 1h, filtering, wherein the temperature of feed liquid during filtering is 18 ℃, obtaining a filter cake which is a creatine monohydrate wet product, and drying to obtain the creatine monohydrate product of 76g in total.
The purity of the creatine monohydrate product is 93.4%, wherein the content of dicyandiamide is less than 20ppm, and the content of creatinine is 5.1%.
In comparison, when hydrochloric acid is dripped into a mixed solution formed by the creatine monohydrate raw material and pure water, the reaction temperature is too high, the quality of the creatine monohydrate product obtained by purification is influenced, and particularly the content of creatinine is obviously increased.
Comparative example 3
The present comparative example provides a method for purifying creatine monohydrate, comprising the steps of:
(1) Taking 100g of creatine monohydrate with the purity of 90%, stirring and mixing with 400g of pure water, then dropwise adding hydrochloric acid with the mass percentage concentration of 30% into the mixture until the creatine monohydrate is completely dissolved, wherein the pH value of a reaction system is 1.5, stopping dropwise adding the hydrochloric acid to obtain a creatine solution, and controlling the temperature of the reaction system to be below 10 ℃ in the hydrochloric acid dropwise adding process;
(2) Adding 0.5g of active carbon into the creatine solution, stirring for 30min, controlling the temperature of a reaction system to be below 10 ℃, and then filtering to obtain filtrate;
(3) And (2) dropwise adding ammonia water with the mass percentage concentration of 20% into the filtrate to adjust the pH value to 7.4, stopping dropwise adding the ammonia water, controlling the temperature of a reaction system to be 28-30 ℃ in the dropwise adding process of the ammonia water, then keeping the temperature and stirring for 1h, filtering, wherein the temperature of feed liquid during filtering is 35 ℃, obtaining a filter cake which is a creatine monohydrate wet product, and drying to obtain a creatine monohydrate product of 73g in total.
The purity of the creatine monohydrate product was 95.3%, with a dicyandiamide content of 3.3% and a creatinine content of less than 50ppm.
The comparison shows that in the process of dropwise adding ammonia water into the filtrate obtained in the step (3), the temperature of a reaction system is controlled to be 28-30 ℃, the temperature is too high, the quality of the creatine monohydrate product obtained by purification is affected, and particularly the content of dicyandiamide is obviously increased.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (10)
1. A method for purifying creatine monohydrate, comprising the steps of:
(1) Mixing creatine monohydrate with water, and then adding acid until the creatine monohydrate is dissolved to obtain a creatine solution;
(2) Adding activated carbon into the creatine solution for treatment, and filtering to obtain filtrate;
(3) And adjusting the pH value of the filtrate to 6-8 by using alkali liquor, and then filtering to obtain a filter cake, namely the creatine monohydrate product.
2. Purification process according to claim 1, characterized in that the creatine monohydrate has a purity of 80-92%, preferably 80-90%.
3. The purification method according to claim 1, characterized in that the creatine monohydrate is mixed with water in a mass ratio of 1: (4-10) mixing, preferably in a mass ratio of 1: (4-6), more preferably mixing in a mass ratio of 1:4, mixing.
4. The purification process according to any one of claims 1 to 3, wherein the acid is hydrochloric acid, preferably the concentration of hydrochloric acid is 28 to 33% by mass, more preferably the concentration of hydrochloric acid is 30% by mass.
5. The purification method according to claim 4, wherein the temperature of the reaction system is controlled to 10 ℃ or lower during the addition of the hydrochloric acid, and/or the addition of the hydrochloric acid is stopped when the pH of the reaction system is 1 to 4.
6. The purification method according to any one of claims 1 to 5, wherein the alkaline solution is ammonia water, preferably the concentration of ammonia water is 15 to 25% by mass, and more preferably the concentration of ammonia water is 20% by mass.
7. The purification method according to claim 6, wherein the temperature of the reaction system is controlled below 10 ℃ during the addition of the alkali solution, and/or the addition of the alkali solution is stopped when the pH is adjusted to 7-8.
8. The purification method according to any one of claims 1 to 7, wherein in the step (3), the temperature of the feed liquid during the filtration is 15 to 20 ℃.
9. The purification method according to any one of claims 1-8, wherein the filter cake is dried to obtain a creatine monohydrate product having a purity of 99.0% or more, wherein the dicyandiamide content is 20ppm or less and the creatinine content is 50ppm or less.
10. Creatine monohydrate product obtainable by the process according to any one of claims 1 to 9.
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| CN106831495A (en) * | 2016-12-28 | 2017-06-13 | 安徽省虹升生物股份有限公司 | A kind of chemical industry synthesis method of creatine monohydrate |
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2022
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|---|---|---|---|---|
| CN1287118A (en) * | 1999-09-07 | 2001-03-14 | 天津天成制药有限公司 | Method of preparing creatine or its hydrate |
| CN101434563A (en) * | 2008-12-15 | 2009-05-20 | 太仓市新毛涤纶化工有限公司 | Preparation of creatine monohydrate |
| CN104086461A (en) * | 2014-07-07 | 2014-10-08 | 上海宝穗化工有限公司 | Preparation method of creatine monohydrate |
| CN106831495A (en) * | 2016-12-28 | 2017-06-13 | 安徽省虹升生物股份有限公司 | A kind of chemical industry synthesis method of creatine monohydrate |
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