CN117550957A - Preparation method of large-particle-size diamond anhydrous inositol crystal - Google Patents
Preparation method of large-particle-size diamond anhydrous inositol crystal Download PDFInfo
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- CN117550957A CN117550957A CN202311429188.7A CN202311429188A CN117550957A CN 117550957 A CN117550957 A CN 117550957A CN 202311429188 A CN202311429188 A CN 202311429188A CN 117550957 A CN117550957 A CN 117550957A
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- inositol
- anhydrous
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- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 title claims abstract description 98
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 title claims abstract description 94
- 229960000367 inositol Drugs 0.000 title claims abstract description 94
- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000013078 crystal Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 13
- 239000010432 diamond Substances 0.000 title claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000654 additive Substances 0.000 claims abstract description 23
- 230000000996 additive effect Effects 0.000 claims abstract description 21
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- SRBFZHDQGSBBOR-HWQSCIPKSA-N L-arabinopyranose Chemical compound O[C@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-HWQSCIPKSA-N 0.000 claims abstract description 6
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims abstract description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 4
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims abstract description 4
- DKXNBNKWCZZMJT-UHFFFAOYSA-N O4-alpha-D-Mannopyranosyl-D-mannose Natural products O=CC(O)C(O)C(C(O)CO)OC1OC(CO)C(O)C(O)C1O DKXNBNKWCZZMJT-UHFFFAOYSA-N 0.000 claims abstract description 4
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims abstract description 4
- 229960002160 maltose Drugs 0.000 claims abstract description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 235000013305 food Nutrition 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 239000003674 animal food additive Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 230000007774 longterm Effects 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 21
- 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 4
- 238000001914 filtration Methods 0.000 description 4
- 241001465754 Metazoa Species 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 125000003599 L-arabinosyl group Chemical group C1([C@H](O)[C@@H](O)[C@@H](O)CO1)* 0.000 description 2
- 235000012000 cholesterol Nutrition 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000399 optical microscopy Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 101100392078 Caenorhabditis elegans cat-4 gene Proteins 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- RFSUNEUAIZKAJO-VRPWFDPXSA-N D-Fructose Natural products OC[C@H]1OC(O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-VRPWFDPXSA-N 0.000 description 1
- BJHIKXHVCXFQLS-UYFOZJQFSA-N D-fructose group Chemical group OCC(=O)[C@@H](O)[C@H](O)[C@H](O)CO BJHIKXHVCXFQLS-UYFOZJQFSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 208000004930 Fatty Liver Diseases 0.000 description 1
- 206010019708 Hepatic steatosis Diseases 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- INAPMGSXUVUWAF-GCVPSNMTSA-N [(2r,3s,5r,6r)-2,3,4,5,6-pentahydroxycyclohexyl] dihydrogen phosphate Chemical compound OC1[C@H](O)[C@@H](O)C(OP(O)(O)=O)[C@H](O)[C@@H]1O INAPMGSXUVUWAF-GCVPSNMTSA-N 0.000 description 1
- 235000004279 alanine Nutrition 0.000 description 1
- 125000003295 alanine group Chemical group N[C@@H](C)C(=O)* 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000032770 biofilm formation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 208000019425 cirrhosis of liver Diseases 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 210000004292 cytoskeleton Anatomy 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000035475 disorder Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 208000010706 fatty liver disease Diseases 0.000 description 1
- 239000003102 growth factor Substances 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 231100000283 hepatitis Toxicity 0.000 description 1
- 229960005436 inositol nicotinate Drugs 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- MFZCIDXOLLEMOO-GYSGTQPESA-N myo-inositol hexanicotinate Chemical compound O([C@H]1[C@@H]([C@H]([C@@H](OC(=O)C=2C=NC=CC=2)[C@@H](OC(=O)C=2C=NC=CC=2)[C@@H]1OC(=O)C=1C=NC=CC=1)OC(=O)C=1C=NC=CC=1)OC(=O)C=1C=NC=CC=1)C(=O)C1=CC=CN=C1 MFZCIDXOLLEMOO-GYSGTQPESA-N 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 238000009374 poultry farming Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000013094 purity test Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000026267 regulation of growth Effects 0.000 description 1
- 230000019491 signal transduction Effects 0.000 description 1
- 231100000240 steatosis hepatitis Toxicity 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 230000001228 trophic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/94—Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
Abstract
The invention provides a preparation method of rhombic anhydrous inositol crystals with large particle size. The preparation method comprises the following steps: under the stirring condition, rapidly cooling the inositol-water mixed solution with the temperature of 60-80 ℃ to 40-60 ℃, then adding an additive, and keeping for 1-4 hours to obtain the rhombic anhydrous inositol crystal with large particle size; the additive comprises any one or a combination of at least two of L-arabinose, D-xylose, D-glucose or D-maltose. The crystallization process has single raw materials, the solvent only involves water, and the method is environment-friendly and has simple process. The diamond anhydrous inositol crystal has uniform particle size and average particle size of 300-500 microns; the product has high fluidity, repose angle of 34-38 degrees, high compressive strength and long-term storage.
Description
Technical Field
The invention belongs to the technical field of chemical engineering industry crystallization, and particularly relates to a preparation method of rhombus anhydrous inositol crystals with large particle sizes.
Technical Field
Inositol, also known as myo-inositol, is a six-carbon cyclic alcohol of formula C 6 H 12 O 6 The sweetness is about 50% of sucrose. Inositol is a substance necessary for the growth of humans, animals and microorganisms, and is called a "growth factor". Inositol, which is a precursor of inositol phosphate and lipid, is involved in various vital activities of the body, such as growth regulation, biofilm formation, signal transduction, etc., and is a human-essential trophic factor.
In the field of medicine, inositol can promote fat metabolism in liver, and can be clinically made into inositol tablet, inositol nicotinate, triglyceride and other medicines for treating liver cirrhosis, fatty liver, hepatitis and other diseases. And simultaneously, inositol can reduce the cholesterol content in blood and treat catabolism disorder of fat and cholesterol. In the food field, inositol is often used as an additive in foods such as health foods, high-grade beverages, dairy products, and the like. More than half of the products are selected to be added with inositol in the full nutrition and infant special medical food, and the inositol can promote the construction of infant cytoskeleton and support the normal development of nervous system and multiple organs of the lung. In the field of feeds, inositol is a necessary nutrient for aquatic animals and has an important role in maintaining normal physiological functions. The application range of the method is expanded to industries such as aquaculture, animal husbandry and poultry farming.
Currently commercial inositol products are mostly in the form of powder and needles with poor crystal morphology. This results in low purity of inositol crystals, severely affecting the organoleptic quality and powder properties of the product. CN 105669376B proposes a crystallization process for preparing high-crystallinity myo-inositol with large grain size, adding 1-5%I myo-inositol crystal nucleus, slowly cooling at 0.1-3 deg.c/hr, and preparing columnar myo-inositol crystal with grain size greater than 100 microns and high crystallinity. However, the length-diameter ratio of the product is too large, which seriously affects the post-treatment process of the product. CN 114181045A proposes a method for preparing spherical anhydrous inositol by using a fluidized bed crystallizer, which improves purity and fluidity of inositol product, but the seed crystal dosage is large (10%), and the obtained spherical polycrystalline crystal is easy to break.
Therefore, finding a preparation method of inositol crystal products which uses a very small amount of seed crystals, greatly improves the crystal particle size and the crystal morphology and can realize industrialization is still a technical problem which cannot be solved by the prior art.
Disclosure of Invention
In order to overcome the defect of poor crystal morphology of the existing inositol product, the invention provides a method for preparing rhombic anhydrous inositol by using an additive, and the prepared rhombic anhydrous inositol crystals have uniform particle size and average particle size of 300-500 microns; the product has high fluidity, repose angle of 34-38 degrees, high compressive strength and long-term storage. Meanwhile, the crystallization process has single raw material, the solvent only relates to water, and the method is environment-friendly and simple in process.
The invention aims at providing a preparation method of rhombus anhydrous inositol crystals, which comprises the following steps:
under the stirring condition, rapidly cooling the inositol-water mixed solution with the temperature of 60-80 ℃ to 40-60 ℃, then adding an additive, and keeping for 1-4 hours to obtain the rhombic anhydrous inositol crystal with large particle size; in the cooling process, the temperature is reduced within the range of 20-30 ℃.
The additive comprises any one or a combination of at least two of L-arabinose, D-xylose, D-glucose or D-maltose.
Preferably, in the inositol-water mixed solution, the concentration of inositol is 0.2-0.5 g/mL.
Preferably, the cooling rate is 4-5 ℃/min.
Preferably, the additive is added in an amount of 1 to 20g based on 100g of the inositol-water solution.
Preferably, the stirring speed is 100-300 rpm;
preferably, the stirred flow field is a flow field formed by anchor paddles or flat angle paddles.
Preferably, the preparation method further comprises the steps of sequentially carrying out solid-liquid separation, cleaning and drying on the mixed solution obtained after the mixed solution is kept for 1-4 hours;
preferably, the solid-liquid separation mode is suction filtration;
preferably, the drying temperature is 40-60 ℃ and the drying time is 4-8h.
The second purpose of the invention is to prepare rhombic anhydrous inositol crystals with large particle size according to the preparation method of the first purpose.
Preferably, the large-particle diamond anhydrous inositol crystal has an average particle size of 300-500 μm.
Preferably, the angle of repose of the large-particle-size rhombic anhydrous inositol crystal is 34-38 degrees;
preferably, the purity of the large-particle diamond anhydrous inositol crystal is 100%.
The third object of the present invention is to provide a rhombohedral anhydrous inositol crystal having a large particle diameter according to the second object for preparing any one of a medicine, a food or a feed additive.
The invention has the technical characteristics and beneficial effects that:
1. according to the method, the morphology of the inositol crystal is effectively improved by adding the additive, and the growth of the dominant crystal face is inhibited by hydrogen bond interaction, so that the rhombic anhydrous inositol crystal is prepared.
2. The diamond anhydrous inositol crystal prepared by the method has the advantages of 300-500 mu m average particle diameter, high purity and good flow property, provides excellent conditions for the subsequent treatment of inositol products, and can reduce the cost and improve the production efficiency.
3. The whole process of the method only uses water as a solvent, has single raw materials, is environment-friendly and simple in process, can realize industrialization and has low economic investment.
Drawings
Fig. 1: optical microscopy pictures of anhydrous inositol starting material;
fig. 2: optical microscopy pictures of diamond-shaped anhydrous inositol crystals;
fig. 3: XRD pattern of anhydrous inositol starting material and rhombohedral anhydrous inositol crystals;
fig. 4: high performance liquid chromatogram of diamond anhydrous inositol crystal;
fig. 5: example 1 particle size distribution of a rhombohedral anhydrous inositol product;
Detailed Description
Example 1:
(1) An inositol-water mixed solution having an inositol concentration of 0.2g/mL was prepared at 60 ℃.
(2) The solution was rapidly cooled to 40℃at 4℃per minute, 1% L-arabinose additive was added thereto, and the mixture was stirred at 300rpm for 1 hour to precipitate crystals.
(3) Filtering, washing and drying at 40 ℃ for 8 hours to obtain diamond anhydrous inositol crystals.
The optical microscope picture of the diamond anhydrous inositol crystal is shown in figure 2, and compared with the anhydrous inositol raw material (figure 1), the crystal morphology is greatly improved. The XRD spectra of the anhydrous inositol raw material and the rhombus anhydrous inositol crystal are shown in figure 3, and the XRD spectra of the anhydrous inositol raw material and the rhombus anhydrous inositol crystal are consistent, so that the prepared rhombus inositol crystal is an anhydrous inositol crystal. The purity test result of the high performance liquid chromatograph is shown in fig. 4, and the purity of the rhombohedral anhydrous inositol crystal in example 1 is 100%. The particle size distribution of the rhombohedral anhydrous inositol crystals in example 1 is shown in fig. 5, and the average particle diameter is 355um and the angle of repose is 34 °.
Example 2:
(1) An inositol-water mixed solution having an inositol concentration of 0.3g/mL was prepared at 70 ℃.
(2) The solution is rapidly cooled to 50 ℃ at 4 ℃/min, 5% of D-xylose additive is added, and the stirring is kept at 200rpm for 2 hours, so that crystals are crystallized and separated out.
(3) Filtering, washing and drying at 50 ℃ for 6 hours to obtain diamond anhydrous inositol crystals.
The diamond-shaped anhydrous inositol crystal obtained in this example was obtained by the same test method as in example 1, and it was found that the obtained diamond-shaped inositol crystal was an anhydrous inositol crystal having a purity of 100%, an average particle diameter of 395 μm, and an angle of repose of 35 °.
Example 3:
(1) An inositol-water mixed solution having an inositol concentration of 0.4g/mL was prepared at 80 ℃.
(2) The solution is rapidly cooled to 60 ℃ at 5 ℃/min, 10% of D-glucose additive is added, and stirring is carried out for 3 hours at 150rpm, so that crystals are crystallized and separated out.
(3) Filtering, washing and drying at 50 ℃ for 6 hours to obtain diamond anhydrous inositol crystals.
The diamond-shaped anhydrous inositol crystal obtained in this example was obtained by the same test method as in example 1, and it was found that the obtained diamond-shaped inositol crystal was an anhydrous inositol crystal having a purity of 100%, an average particle diameter of 445 μm and an angle of repose of 36 °.
Example 4:
(1) An inositol-water mixed solution having an inositol concentration of 0.5g/mL was prepared at 80 ℃.
(2) The solution is rapidly cooled to 60 ℃ at 5 ℃/min, 20% of D-maltose additive is added, and stirring is carried out for 4 hours at 100rpm, so that crystals are crystallized and separated out.
(3) Filtering, washing and drying at 40 ℃ for 8 hours to obtain diamond anhydrous inositol crystals.
The diamond-shaped anhydrous inositol crystal obtained in this example was obtained by the same test method as in example 1, and it was found that the obtained diamond-shaped inositol crystal was an anhydrous inositol crystal having a purity of 100%, an average particle diameter of 486um, and an angle of repose of 38 °.
Comparative example 1:
the difference from example 1 is only that 0.1% L-arabinose additive was added in step (2), and the rest of the preparation method was the same as in example 1.
No rhombic anhydrous inositol crystal is obtained in the comparative example, and the morphology of the crystal is long needle-shaped.
As is clear from comparative examples 1 and 1, when the addition amount of the additive is below the limit of the present invention, the hydrogen bond interaction between the groups is weak, the morphology of the crystals is long needle-like, and rhombohedral anhydrous inositol crystals cannot be formed.
Comparative example 2:
the difference from example 1 is only that 30% L-arabinose additive was added in step (2), and the rest of the preparation method was the same as in example 1.
No rhombic anhydrous inositol crystal is obtained in the comparative example, and the morphology of the crystal is long needle-shaped.
As is clear from comparative examples 1 and 2, when the amount of the additive added exceeds the range defined in the present invention, the solution system becomes viscous and forms a paste-like morphology, giving the inositol crystal morphology of long needles.
Comparative example 3:
the difference from example 1 was that the stirring rate in step (2) was 500rpm, and the other preparation methods were the same as in example 1.
The comparative example did not give rhombohedral anhydrous inositol crystals, which were long needle-like in morphology and severely crushed.
As is clear from comparative examples 1 and 3, when the stirring rate exceeds the limit of the present invention, the collision between crystals is increased, resulting in breakage of crystals and serious influence on the morphology of inositol crystals.
Comparative example 4:
the difference from example 1 is that L-arabinose was replaced with D-fructose, and the other preparation methods were the same as in example 1.
No rhombic anhydrous inositol crystal is obtained in the comparative example, and the morphology of the product is long needle-shaped.
As is clear from comparative examples 1 and 4, diamond-shaped crystals of anhydrous inositol could not be obtained when the additive types exceeded the limit of the present invention.
Comparative example 5:
the difference from example 1 is that L-arabinose was replaced with alanine, and the other preparation methods were the same as in example 1.
No rhombic anhydrous inositol crystal is obtained in the comparative example, and the morphology of the product is long needle-shaped.
As is clear from comparative examples 1 and 5, diamond-shaped crystals of anhydrous inositol could not be obtained when the additive types exceeded the limit of the present invention.
Comparative example 6
The only difference from example 3 is that the temperature was reduced to 70℃and the rest of the preparation was identical to example 3.
The solution in this comparative example was always in a clear state, and no rhombohedral anhydrous inositol crystals were obtained.
As is clear from comparative examples 1 and 5, a temperature decrease range below the range defined in the present invention results in too low supersaturation of the mixed solution and no crystal formation.
Comparative example 7
The only difference from example 3 is that the temperature was reduced to 30℃and the rest of the preparation was identical to example 3.
The comparative example gives a mixed product of rhombic anhydrous inositol crystals and long needle-shaped anhydrous inositol crystals.
As is clear from comparative examples 1 and 6, when the temperature reduction interval is higher than the limit range of the present invention, the supersaturation degree of the mixed solution is too high, and a large amount of needle-like crystals are generated, which affects the quality of the product.
The invention discloses and provides a preparation method of large-particle-size rhombic anhydrous inositol crystals. Those skilled in the art can properly change the links of the temperature of the mixed solution, the concentration of inositol, the types of the additives, the addition amount of the additives, the stirring rate and the like by referring to the content of the present disclosure. While the method of the present invention has been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that variations and combinations of the methods and products described herein can be made to practice the present technology without departing from the spirit or scope of the invention. It is expressly noted that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be included within the spirit, scope and content of the invention.
Claims (10)
1. The preparation method of the rhombic anhydrous inositol crystal with large particle size is characterized by comprising the following steps:
under the stirring condition, rapidly cooling the inositol-water mixed solution with the temperature of 60-80 ℃ to 40-60 ℃, then adding an additive, and keeping for 1-4 hours to obtain the rhombic anhydrous inositol crystal with large particle size;
the additive comprises any one or a combination of at least two of L-arabinose, D-xylose, D-glucose or D-maltose.
2. The method according to claim 1, wherein the concentration of inositol in the inositol-water mixed solution is 0.2 to 0.5g/mL.
3. The method according to claim 1, wherein the cooling rate is 4-5 ℃/min.
4. The method according to claim 1, wherein the additive is added in an amount of 1 to 20g based on 100g of the inositol-water solution.
5. The method according to claim 1, wherein the stirring speed is 100 to 300rpm;
preferably, the stirred flow field is a flow field formed by anchor paddles or flat angle paddles.
6. The method according to claim 1, further comprising subjecting the mixed solution obtained after holding for 1 to 4 hours to solid-liquid separation, washing and drying in this order;
preferably, the solid-liquid separation mode is suction filtration;
preferably, the drying temperature is 40-60 ℃ and the drying time is 4-8h.
7. The process according to any one of claims 1 to 6, wherein large-particle diamond-shaped anhydrous inositol crystals are obtained.
8. The large-particle diameter rhombohedral anhydrous inositol crystal according to claim 7, wherein the average particle diameter of the large-particle diameter rhombohedral anhydrous inositol crystal is 300 to 500 μm.
9. The large-particle diameter rhombohedral anhydrous inositol crystal according to claim 7, wherein the repose angle of the large-particle diameter rhombohedral anhydrous inositol crystal is 34 to 38 °;
preferably, the purity of the large-particle diamond anhydrous inositol crystal is 100%.
10. The large-particle diameter rhombohedral anhydrous inositol crystal according to claim 7, which is used for preparing any one of a medicine, a food or a feed additive.
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