CN1034013C - Preparing process for rich maleic acid rare-earth complex - Google Patents

Preparing process for rich maleic acid rare-earth complex Download PDF

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Publication number
CN1034013C
CN1034013C CN93110253A CN93110253A CN1034013C CN 1034013 C CN1034013 C CN 1034013C CN 93110253 A CN93110253 A CN 93110253A CN 93110253 A CN93110253 A CN 93110253A CN 1034013 C CN1034013 C CN 1034013C
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China
Prior art keywords
rare
fumaric acid
earth complex
maleic acid
earth
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Expired - Fee Related
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CN93110253A
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CN1074675A (en
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金美荣
刘军
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CHEMICAL RESEARCH INST SHANDONG PROV
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CHEMICAL RESEARCH INST SHANDONG PROV
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Abstract

The present invention relates to a method for preparing fumaric acid rare-earth complex for a feed supplement. Fumaric acid and rare earth chloride are used as raw materials to directly react. The reaction time is from 1 to 2 hours, the reaction temperature is from 20 to 60 DEG C, and the optimum reaction temperature is from 40 to 45 DEG C. Deionized water is used as a solvent, and the yield is more than 75%. The fumaric acid rare-earth complex is used as the feed supplement.

Description

A kind of preparation method of rich maleic acid rare-earth complex
The invention relates to the preparation method of rich maleic acid rare-earth complex, particularly belong to sodium fumarate and lanthanon, lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, the method field of the synthetic rich maleic acid rare-earth complex of muriate reaction of samarium Sm.
China's rare earth resources is abundant, rich maleic acid rare-earth complex, in fodder industry, use and have bright prospects, because rich maleic acid rare-earth has dual function, the one, fumaric acid itself is the sanitas in the foodstuff additive, the 2nd, rare earth ion has the growth effect that promotes animal, thereby the research of exploitation rich maleic acid rare-earth complex, and being needs the problem that solves in the present feed industry.
About the preparation method of rich maleic acid rare-earth complex, Polish scholar Brzyska in 1973, Wanda etc. are just relevant for the detailed introduction of having been undertaken reporting (C.A.88:1520Sm) by ammonium fumarate and the directly synthetic rich maleic acid rare-earth of rare earth chloride but not seen this method.The by product of the synthetic rich maleic acid rare-earth of ammonium fumarate and rare earth chloride is an ammonium chloride, and as fodder additives, ammonium chloride is objectionable impurities, can not use.
Purpose of the present invention is exactly to seek a kind of preparation method of the rich maleic acid rare-earth complex that uses as fodder additives.
In order to realize purpose of the present invention, the inventor adopts the muriate reaction of sodium fumarate and lanthanon (lanthanum, cerium, praseodymium, neodymium, samarium) to synthesize rare-earth complexs such as fumaric acid lanthanum, fumaric acid cerium, fumaric acid praseodymium, fumaric acid neodymium, fumaric acid samarium, it is solvent that sodium fumarate and lanthanide chloride adopt water, reaction times is 1-2 hour, temperature of reaction is 20 to 60 ℃, its best temperature of reaction is 40 to 45 ℃, and reaction product is dry under 105-110 ℃, and yield is 75 to 88%.
The molecular formula of rich maleic acid rare-earth complex of the present invention is:
Ln 2(C 4H 2O 4) 3·nH 2O (1)
(1) Ln in the formula represents rare earth element
Sodium fumarate and rare earth chloride reaction generate the reactional equation of rich maleic acid rare-earth complex and are represented by following equation:
(2)
Sodium fumarate of the present invention is that with the advantage of the rich maleic acid rare-earth complex that the muriate reaction of lanthanon generates the by product sodium-chlor that reacts generation separates with product, and nontoxic easily, can make fodder additives and use.
The present invention be suitable for equally sodium fumarate and lanthanon gadolinium, dysprosium, erbium, ytterbium, lutetium (Gd, Dy, Er, Yb, corresponding muriate reaction such as Lu) obtains complex compounds such as fumaric acid gadolinium, fumaric acid dysprosium, fumaric acid erbium, fumaric acid ytterbium, fumaric acid lutetium.Enumerate several embodiment below, further specify the present invention.
Embodiment:
Example 1:
Stirring is being housed, in the there-necked flask of thermometer and water cooler, is adding 24.0 gram sodium fumarates and 24.5 gram Lanthanum trichlorides, adding 300 milliliters of deionized waters, stirring, heating up gradually is heated to 60 ℃, stirs after 2 hours, stops.Pour out product, cooling, filter, with small amount of ethanol and water washing product, 105 °-110 ℃ dry down, dry product 23.5 grams, yield 75.8%.
Fumaric acid lanthanum molecular formula: La 2(C 4H 2O 4) 32H 2O, elementary composition; Theoretical value: C 21.97% H 1.54% La 42.35% measured value: C22.06% H 1.78% La 42.79%
Example 2:
In example 1 device, add 24.0 gram sodium fumarates and 24.7 gram cerous chlorates, add 300 ml deionized water, be heated to 50 ℃, stirring reaction stopped in 2 hours, pour out product, cooled and filtered, with small amount of ethanol and water washing product, dry down at 105-110 ℃, get dry product 25.2 grams, yield 81.0%.
Fumaric acid cerium Ce 2(C 4H 2O 4) 32H 2O
Elementary composition; Theoretical value: C 21.30% H 1.49% Ce 41.43%
Measured value: C 21.51% H 1.56% Ce 41.60%
Example 3:
In example 1 device, add 24.0 gram sodium fumarates, 24.7 gram praseodymium chloride and 300 ml deionized water are heated to 50 ℃, stirring reaction stopped after 2 hours, poured out the reaction product cooling, filtered, with small amount of ethanol and water washing product, dry that fumaric acid praseodymium dry product 25.2 restrains yield 80.8%.
Pr 2(C 4H 2O 4) 3·2H 2O
Elementary composition; Theoretical value: C 21.84% H 1.53% Pr 42.70%
Measured value: C 21.88% H 1.68%% Pr 43.00%
Example 4:
In example 1 device, add 24.0 gram sodium fumarates, 25.1 gram Neodymium trichloride and 300 ml deionized water are heated to 40 ℃, stirring reaction stopped after 1 hour, poured out product, after the cooling, filtered, with small amount of ethanol and water washing product, dry that fumaric acid neodymium dry product 27.7 restrains yield 87.8%.
Nd 2(C 4H 2O 4) 3·2H 2O
Elementary composition; Theoretical value: C 21.62% H 1.51% Nd 43.28%
Measured value: C 21.80% H 1.61% Nd 43.42%
Example 5:
Add 24.0 gram sodium fumarates in example 1 device, 25.7 gram samarium trichloride and 300 ml deionized water are heated to 45 ℃, stirring reaction stopped after 1 hour, pour out product, cooling, filtration, use small amount of ethanol and water washing product, dry that fumaric acid samarium dry product 28.4 restrains yield 88.3%.
Sm 2(C 4H 2O 4) 3·2H 2O
Elementary composition; Theoretical value: C 21.22% H 1.48% Sm 44.31%
Measured value: C 21.33% H 1.56% sm 43.42%

Claims (4)

1. the preparation method of a rich maleic acid rare-earth complex is characterized in that:
A. adopting sodium fumarate and rare earth chloride is raw material,
B. adopting deionized water is solvent,
C. temperature of reaction is 20 to 60 ℃,
D. Fan Ying time is 1 to 2 hour.
2. the preparation method of a kind of rich maleic acid rare-earth complex according to claim 1 is characterized in that described temperature of reaction is 40 to 45 ℃.
3. the preparation method of a kind of rich maleic acid rare-earth complex according to claim 1 is characterized in that said rare earth chloride is Lanthanum trichloride, cerous chlorate, praseodymium chloride, Neodymium trichloride, samarium trichloride.
4. the preparation method of a kind of rich maleic acid rare-earth complex according to claim 1 is characterized in that described preparation method comprises the preparation method of fumaric acid lanthanum, fumaric acid cerium, fumaric acid praseodymium, fumaric acid neodymium, fumaric acid samarium rare-earth complex.
CN93110253A 1993-01-19 1993-01-19 Preparing process for rich maleic acid rare-earth complex Expired - Fee Related CN1034013C (en)

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CN93110253A CN1034013C (en) 1993-01-19 1993-01-19 Preparing process for rich maleic acid rare-earth complex

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CN1074675A CN1074675A (en) 1993-07-28
CN1034013C true CN1034013C (en) 1997-02-12

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2130300A1 (en) * 1971-06-18 1972-12-21 Chemie Linz Ag Fumarate prepn from maleates - by heating with ammonium chloride or carbonate as catalyst
CN88102641A (en) * 1988-04-29 1988-12-07 吕福森 Fatty acid rare earth compound and its technology

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2130300A1 (en) * 1971-06-18 1972-12-21 Chemie Linz Ag Fumarate prepn from maleates - by heating with ammonium chloride or carbonate as catalyst
CN88102641A (en) * 1988-04-29 1988-12-07 吕福森 Fatty acid rare earth compound and its technology

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