CN102367224B - Method for preparing calcium fumarate or zinc fumarate - Google Patents
Method for preparing calcium fumarate or zinc fumarate Download PDFInfo
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- CN102367224B CN102367224B CN201110339486.8A CN201110339486A CN102367224B CN 102367224 B CN102367224 B CN 102367224B CN 201110339486 A CN201110339486 A CN 201110339486A CN 102367224 B CN102367224 B CN 102367224B
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- fumaric acid
- zinc
- calcium
- fumarate
- chloride
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- HJSYJHHRQVHHMQ-TYYBGVCCSA-L zinc;(e)-but-2-enedioate Chemical compound [Zn+2].[O-]C(=O)\C=C\C([O-])=O HJSYJHHRQVHHMQ-TYYBGVCCSA-L 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 23
- RWYRUDPAALLKPX-UHFFFAOYSA-N 2,2-difluoro-n-methylethanamine;hydrochloride Chemical compound Cl.CNCC(F)F RWYRUDPAALLKPX-UHFFFAOYSA-N 0.000 title abstract 4
- 239000001749 Calcium fumarate Substances 0.000 title abstract 4
- 235000019296 calcium fumarate Nutrition 0.000 title abstract 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims abstract description 60
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000001530 fumaric acid Substances 0.000 claims abstract description 30
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000011575 calcium Substances 0.000 claims abstract description 13
- 239000001110 calcium chloride Substances 0.000 claims abstract description 13
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 13
- 239000011701 zinc Substances 0.000 claims abstract description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 239000011592 zinc chloride Substances 0.000 claims abstract description 7
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- HDRTWMBOUSPQON-TYYBGVCCSA-L calcium;(e)-but-2-enedioate Chemical compound [Ca+2].[O-]C(=O)\C=C\C([O-])=O HDRTWMBOUSPQON-TYYBGVCCSA-L 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229910001868 water Inorganic materials 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- IPCXNCATNBAPKW-UHFFFAOYSA-N zinc;hydrate Chemical compound O.[Zn] IPCXNCATNBAPKW-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000243 solution Substances 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 150000001298 alcohols Chemical class 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009469 supplementation Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 230000029663 wound healing Effects 0.000 description 2
- 208000010470 Ageusia Diseases 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- -1 Fumarate ion Chemical class 0.000 description 1
- 206010020989 Hypogeusia Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000012628 flowing agent Substances 0.000 description 1
- 235000019570 hypogeusia Nutrition 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000014860 sensory perception of taste Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 230000004102 tricarboxylic acid cycle Effects 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- GLHGFMYBJKLJFS-UHFFFAOYSA-N zinc azanide dichloroazanide Chemical compound ClN([Zn]N)Cl GLHGFMYBJKLJFS-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing calcium fumarate or zinc fumarate. The method comprises the following steps: (1) mixing fumaric acid and ammonia water to prepare a mixed solution; (2) preparing a calcium chloride or zinc chloride solution; (3) mixing the mixed solution prepared in step (1) with the calcium chloride or zinc chloride solution prepared in step (2), and carrying out stirring, cooling, crystallization, pumping filtration, rinsing and drying to prepare calcium fumarate or zinc fumarate. The method provided in the invention can be used for preparation of the pure substance of calcium fumarate (fumaric acid:calcium = 1:1) or zinc fumarate (fumaric acid:zinc = 1:1). The method has the following advantages: organic solvents like alcohols and acetic acid are not used, being environment friendly; drying is realized by direct utilization of a common baking oven without need for microwave or spray drying or the like, thereby reducing energy consumption.
Description
Technical field
The invention belongs to chemical field, relate to a kind of method of preparing Fumaric acid, calcium salt or zinc fumarate.
Background technology
By fumaric acid (H
2c
4h
2o) be combined with zine ion form organic zinc source fodder additives zinc fumarate there is bioactive material as one, added in feed, there is mildew-resistant, antibacterial, improve the effects such as efficiency of feed utilization and livestock and poultry production performance, have simultaneously non-stimulated, absorb the features such as fast, belong to a kind of animal zinc supplementation reinforcer of excellent property.Fumarate ion in zinc fumarate can participate in tricarboxylic acid cycle, forms ATP required for organism metabolism, can be used as carbon skeleton synthesizing amino acid, the one-step synthesis albumen of going forward side by side.
Zinc is the essential one trace element of humans and animals, having accelerating growth grows, improves the sense of taste, regulates human body immunity, protect from infection and promote the functions such as wound healing, the serious problems such as scarce zinc can cause cessation of growth cessation, and Idiopathic hypogeusia and wound healing are bad, thus various diseases caused.Due to the peculiar biochemical property of fumaric acid, the zinc fumarate forming of being combined with zine ion has nonirritant, it is fast to absorb, bioavailability is high, also has the dual function of mildew-resistant and treatment, is a kind of zinc supplementation reinforcer of excellent property.
Fumaric acid, calcium salt can be used as the function of anti-caking agent or flowing agent.Also can be used as the additive of replenishing the calcium.
1) and pair Fumaric acid, calcium salt (fumaric acid: calcium=2: the 1) method of mixture at present it prepares the preparation method (referring to patent CN88104750.3 and CN97104808.8) of the Fumaric acid, calcium salt of report is a kind of Fumaric acid, calcium salt (fumaric acid: calcium=1:.Because alkali and the solubleness of product Fumaric acid, calcium salt in water of fumaric acid, calcium are all smaller, so direct reaction cannot be prepared pure Fumaric acid, calcium salt (fumaric acid: calcium=1: 1) wherein even also have the not fumaric acid of complete reaction and the alkali of calcium.
The preparation method of the zinc fumarate of report at present:
(1) research of fodder additives zinc fumarate new preparation process (fodder industry desolate do flat Chen Zhichuan): add ammonium chloride in the aqueous solution of water or containing ammonium chloride, then add secondary zinc oxide solid to carry out neutrality leaching; Adopt the method for hydrogen peroxide oxidation deironing and zinc powder segmented replacement deleading, cadmium, copper to remove all dirt; Crystallization; Gained dichloro diamino zinc is mixed by equimolar amount with fumaric acid, be then poured into water stirring reaction, then filter, filter cake is washed with pure water, dry to obtain zinc fumarate.
(2) reaction process that cis-butenedioic anhydride one still process catalyzes and synthesizes zinc fumarate (Jiang Yizhong, Materials Physics and Chemistry (specialty) Ph D dissertation) the method is divided into two stages:
Stage one is isomerization reaction: in 3 mouthfuls of flasks that mechanical stirring and reflux exchanger are housed, add MALEIC ANHYDRIDE, catalyst A and the distilled water of metering, stirring heating makes to be micro-boiling; After backflow certain hour (2.5h), draw a small amount of reaction solution cold filtration in flask, draw a certain amount of filtrate mensuration acid number and determine reaction end.
Stage two is zinc salt building-up process:
In the there-necked flask of determining after stage one reaction end, add zn cpds and the catalyst B of metering, continue stirring heating and make to be micro-boiling; After backflow certain hour (2h), in absorption flask, a small amount of solid matter is cooling, takes a certain amount of white solid that blots residual solution with filter paper; Add with filtering in standard solution of sodium hydroxide and after the 95% ethanol jolting 10min crossing, filtrate being used for measured acid number to determine reaction end, determine reactant after terminal through cooling, filter (filtrate does not discard, can reuse), dry, get product.
Note: acid anhydrides: (catalyst A+catalyst B)=1: (0.06+0.0045) (mol ratio)
(3) Synthesis of zinc fumarate by solid phase reaction under microwave irradiation (Yang Xin is refined, application chemical industry the 9th phase in 2005): by fumaric acid and Zn (CH
3cOO)
22H
2o, in agate mortar, adds a small amount of 95% ethanol, at room temperature fully grinds, and be then under 600W condition, to be radiated to acetic acid taste to disappear to the greatest extent at microwave power.Cooling, with absolute ethanol washing, dry, obtain white solid.
The technical scheme cost that prior art is prepared zinc fumarate is high, and step complexity needs to use a large amount of organic solvents to be unfavorable for environmental protection in preparation process!
Summary of the invention
The object of the present invention is to provide a kind of method of preparing Fumaric acid, calcium salt or zinc fumarate.
Object of the present invention can be achieved through the following technical solutions:
Prepare a method for Fumaric acid, calcium salt or zinc fumarate, it is to comprise the following steps: (1) gets fumaric acid and ammoniacal liquor mixes, and makes mixed solution; (2) prepare calcium chloride or liquor zinci chloridi; (3) calcium chloride prepared by the mixed solution of being prepared by step (1) and step (2) or liquor zinci chloridi mix, stir crystallisation by cooling, separate and obtain Fumaric acid, calcium salt or zinc fumarate.
The above-mentioned method of preparing Fumaric acid, calcium salt or zinc fumarate, its pH value that is described ammoniacal liquor is 6～8, the mass volume ratio (g: ml) of fumaric acid and ammoniacal liquor is: 1: 1.5～2.5, the mol ratio of fumaric acid and calcium chloride or zinc chloride is 1: 1.
The above-mentioned method of preparing Fumaric acid, calcium salt or zinc fumarate, it is described calcium chloride or mass percentage concentration >=10% of liquor zinci chloridi.
The above-mentioned method of preparing Fumaric acid, calcium salt or zinc fumarate, its preparation method who is described calcium chloride solution is: get calcium oxide or calcium carbonate, water and concentrated hydrochloric acid mixing and make; Or directly getting calcium chloride is dissolved in water and obtains.
The above-mentioned method of preparing Fumaric acid, calcium salt or zinc fumarate, its preparation method who is described liquor zinci chloridi is: get zinc oxide, water and concentrated hydrochloric acid mixing and make; Or directly getting zinc chloride is dissolved in water and obtains.
The above-mentioned method of preparing Fumaric acid, calcium salt or zinc fumarate, it is its fumaric acid of prepared Fumaric acid, calcium salt: calcium mol ratio is 1: 1.
The above-mentioned method of preparing Fumaric acid, calcium salt or zinc fumarate, it is its fumaric acid of prepared zinc fumarate: zinc mol ratio is 1: 1.
Beneficial effect of the present invention:
1) or zinc fumarate (fumaric acid: zinc=1: 1) pure substance, quality product is high, pure inclusion-free 1. can prepare Fumaric acid, calcium salt (fumaric acid: calcium=1:.
2. not with an organic solvent as alcohols, acetic acid etc., safe environmentally safe.
3. can reduce energy consumption, not need microwave or spraying dry etc., directly a conventional oven is dry.
4. preparation method is simple, and cost is low.
Embodiment
Embodiment 1 prepares Fumaric acid, calcium salt:
In 1000ml beaker, adding 232g fumaric acid and pH value is 6～8 ammoniacal liquor 464ml, and stir solids is all dissolved.Filter and remove micro-insolubles, stand-by.
In another 1000ml beaker, add 112g calcium oxide or 200g calcium carbonate, 300ml water, concentrated hydrochloric acid 332ml, stir solids is all dissolved, and makes calcium chloride solution.
In 2000ml beaker, above-mentioned two kinds of feed liquids are mixed, stir crystallisation by cooling, separate out Fumaric acid, calcium salt.Suction filtration, washing, oven dry, make qualified product.Detected result is in table 1.
Embodiment 2 prepares Fumaric acid, calcium salt:
In 1000ml beaker, adding 232g fumaric acid and pH value is 6～8 ammoniacal liquor 580ml, and stir solids is all dissolved.Filter and remove micro-insolubles, stand-by.
In another 1000ml beaker, add 222g calcium chloride and 518ml water, be stirred to solid and all dissolve, make mass percentage concentration and be 30% calcium chloride solution.
In 2000ml beaker, above-mentioned two kinds of feed liquids are mixed, stir crystallisation by cooling, separate out Fumaric acid, calcium salt.Suction filtration, washing, oven dry, make qualified product.Detected result is in table 1.
Embodiment 3 prepares zinc fumarate:
In 1000ml beaker, adding 232g fumaric acid and pH value is 6～8 ammoniacal liquor 464ml, and stir solids is all dissolved.Filter and remove micro-insolubles, stand-by.
In another 1000ml beaker, add 162g zinc oxide, 300ml water, concentrated hydrochloric acid 332ml, stir solids is all dissolved, and makes liquor zinci chloridi.
In 2000ml beaker, above-mentioned two kinds of feed liquids are mixed, stir crystallisation by cooling, separate out zinc fumarate.Suction filtration, washing, oven dry, make qualified product.Detected result is in table 2.
Embodiment 4 prepares zinc fumarate:
In 1000ml beaker, adding 232g fumaric acid and pH value is 6～8 ammoniacal liquor 580ml, and stir solids is all dissolved.Filter and remove micro-insolubles, stand-by.
In another 1000ml beaker, add 272g zinc chloride, 634ml water, stir solids is all dissolved, and makes mass percentage concentration and be 30% liquor zinci chloridi.
In 2000ml beaker, above-mentioned two kinds of feed liquids are mixed, stir crystallisation by cooling, separate out zinc fumarate.Suction filtration, washing, oven dry, make qualified product.Detected result is in table 2.
The quality examination result of Fumaric acid, calcium salt prepared by table 1 embodiment 1 and embodiment 2
| Project | Index | Embodiment 1 | Embodiment 2 |
| Outward appearance | White crystalline powder | White powder | White powder |
| Heavy metal (Pb) | ≤20ppm | ＜20ppm | ＜20ppm |
| Sulfate radical (SO 4 2-) | ≤0.01％ | ＜0.01％ | ＜0.01％ |
| Maleic acid | ≤0.05％ | ＜0.05％ | ＜0.05％ |
| Weight loss on drying | ≤0.50％ | 0.12％ | 0.11％ |
| Calcium (Ca 2+) | 25％-27％ | 26.02％ | 26.01％ |
| Content | 98.0％-102％ | 99.87％ | 99.91％ |
| PH | 5-7 | 5.81 | 5.89 |
| Qualified | Qualified |
The quality examination result of zinc fumarate prepared by table 2 embodiment 3 and embodiment 4
| Project | Index | Embodiment 3 | Embodiment 4 |
| Outward appearance | White crystalline powder | White powder | White powder |
| Heavy metal (Pb) | ≤20ppm | ＜20ppm | ＜20ppm |
| Maleic acid | ≤0.05％ | ＜0.05％ | ＜0.05％ |
| Weight loss on drying | ≤5.0％ | 0.55％ | 0.52％ |
| Zinc (Zn 2+) | 35.5％-37.5％ | 36.44％ | 36.31％ |
| Content | 98.0％-102％ | 98.87％ | 99.12％ |
| PH | 4-7 | 5.02 | 5.10 |
| Qualified | Qualified |
Result shows: prepared Fumaric acid, calcium salt, and the mol ratio of fumaric acid and calcium is 1: 1, quality product is high, pure inclusion-free.Prepared zinc fumarate, the mol ratio of fumaric acid and zinc is 1: 1, quality product is high, pure inclusion-free.
Claims (3)
1. prepare a method for Fumaric acid, calcium salt or zinc fumarate, it is characterized in that comprising the following steps: (1) gets fumaric acid and ammoniacal liquor mixes, and makes mixed solution; (2) prepare calcium chloride or liquor zinci chloridi; (3) calcium chloride prepared by the mixed solution of being prepared by step (1) and step (2) or liquor zinci chloridi mix, stir crystallisation by cooling, separate and obtain Fumaric acid, calcium salt or zinc fumarate; The pH value of described ammoniacal liquor is 6 ~ 8, and the mass volume ratio g:ml of fumaric acid and ammoniacal liquor is: 1:1.5 ~ 2.5, and the mol ratio of fumaric acid and calcium chloride or zinc chloride is 1:1; Described calcium chloride or mass percentage concentration >=10% of liquor zinci chloridi; The preparation method of described calcium chloride solution is: get calcium oxide or calcium carbonate, water and concentrated hydrochloric acid mixing and make; Or directly getting calcium chloride is dissolved in water and obtains; The preparation method of described liquor zinci chloridi is: get zinc oxide, water and concentrated hydrochloric acid mixing and make; Or directly getting zinc chloride is dissolved in water and obtains.
2. the method for preparing Fumaric acid, calcium salt or zinc fumarate according to claim 1, is characterized in that its fumaric acid of prepared Fumaric acid, calcium salt: calcium mol ratio is 1:1.
3. the method for preparing Fumaric acid, calcium salt or zinc fumarate according to claim 1, is characterized in that its fumaric acid of prepared zinc fumarate: zinc mol ratio is 1:1.
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| CN107373144B (en) * | 2017-08-22 | 2021-01-01 | 南宁市泽威尔饲料有限责任公司 | Zinc fumarate complex and preparation method and application thereof |
| CN107473956B (en) * | 2017-08-29 | 2021-01-05 | 南京雪郎化工科技有限公司 | Production method of ferrous fumarate |
| CN111138271A (en) * | 2020-01-20 | 2020-05-12 | 太原理工大学 | Preparation method of organic metal salt additive |
| CN112538011A (en) * | 2020-12-23 | 2021-03-23 | 河南瑞贝佳生物科技有限公司 | Preparation method of calcium fumarate |
| CN117563557B (en) * | 2023-11-03 | 2024-10-11 | 江苏海普功能材料有限公司 | Defluorination adsorbent, preparation method thereof and defluorination method of lithium battery recovery liquid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040023A (en) * | 1987-07-31 | 1990-02-28 | 通用食品公司 | Preparation for rapidly solubilized calcium fumarate |
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