CN102952060A - Preparation method of feed additive tryptophane copper complex - Google Patents
Preparation method of feed additive tryptophane copper complex Download PDFInfo
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- CN102952060A CN102952060A CN2012105092852A CN201210509285A CN102952060A CN 102952060 A CN102952060 A CN 102952060A CN 2012105092852 A CN2012105092852 A CN 2012105092852A CN 201210509285 A CN201210509285 A CN 201210509285A CN 102952060 A CN102952060 A CN 102952060A
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Abstract
The invention relates to a preparation method of feed additive tryptophane copper complex, which belongs to the technical field of feed additive preparation and aims at solving the problems that in the existing preparation method, the reaction time is long, the reaction process is difficult to control, the product yield is low, the product purity is low, and the like. The preparation method comprises the following steps of using inorganic copper salt solution and tryptophane solution as raw materials, wherein copper salt is excessive; reacting under the conditions that the pH (Potential of Hydrogen) is 7.5-8.2 and the temperature is 80-100 DEG C by adding the inorganic copper salt solution into the tryptophane solution in a dripping way; and then cooling, separating and drying, thus obtaining a product. The preparation method disclosed by the invention has the advantages that the reaction speed is obviously increased, the yield and the purity of the tryptophane copper complex are both obviously increased, the step is simple, the operation is easy, and the reaction is stable.
Description
Technical field
The present invention relates to the copper complex formazan preparation method of a kind of fodder additives tryptophane, belong to the preparing technical field of fodder additives.
Background technology
Tryptophane copper complex fodder additives belongs to third generation microelement feed addictive----amino-acid trace element copper complex.
The tryptophane copper complex be at home and abroad develop faster in recent years, state-of-the art fodder additives, it is the essential copper metal ion of animal and indispensable amino acid---the complex compound with ring texture or inner complex that-color base acid-respons generates.Because its copper supplement close to natural form in the animal body, and have the characteristics such as good chemical stability, higher biological value, absorption easy to digest, anti-interference, non-stimulated, toxicological harmless effect.Be considered at present a kind of ideal copper additives.
The copper complex formazan method of existing preparation tryptophane, the existence reaction is slow, yield is low, purity is low, reaction process is difficult to the problems such as control.
Summary of the invention
In order to address the above problem, the present invention has fully studied the copper complex formazan physicochemical property of tryptophane according to the exploration of for many years research and production practice, has found out a kind of simple, copper complex formazan preparation method of fodder additives tryptophane.
The copper complex formazan preparation method of a kind of fodder additives tryptophane comprises the steps:
(1) according to the inorganic mantoquita of 1.05-1.3mol: the ratio of 2mol tryptophane is prepared raw material;
(2) with deionized water inorganic mantoquita is dissolved fully preparation Inorganic Copper salts solution;
(3) tryptophane is dissolved with sodium hydroxide solution, preparation pH is the tryptophane solution of 7.6-8.2;
(4) tryptophane solution is heated to 80-100 ℃, constant temperature continues to stir, and drips the Inorganic Copper salts solution to it, and 0.5-1h dropwises; Stir speed (S.S.) is 65-125r/min;
(5) be cooled to 20-40 ℃ after dropwising, then separate, drying, both product.
Above-mentioned preparation method, preferred, the mol ratio of described inorganic mantoquita and tryptophane is 1.1-1.2:2.
Above-mentioned preparation method, preferred, the temperature of described tryptophane solution is 85-95 ℃.
Above-mentioned preparation method, preferred, the pH of described tryptophane solution is 7.9-8.
Above-mentioned preparation method, preferred, the rate of addition of the front 75%-90% of Inorganic Copper salts solution is 2-4 times of afterwards rate of addition; Described percentage ratio is percent by volume.
Above-mentioned preparation method, preferred, stir speed (S.S.) is 65-85r/min.
Preparation method of the present invention, its raw material adopts Inorganic Copper salts solution and alkaline tryptophane solution; After tryptophane solution and the Inorganic Copper salt solution mix, the rapid complexing of the tryptophane molecule of free state and cupric ion forms the tryptophane copper complex; Compare and adopt solid-state inorganic mantoquita or tryptophane crystal, its speed of reaction obviously improves.Simultaneously, reaction adopts the mode that the Inorganic Copper salts solution is added drop-wise in the tryptophane solution to carry out; When making the cupric ion of each adding and tryptophan reaction, tryptophane is excessive; Therefore cupric ion can both with three tryptophane molecular complex; Thereby the copper complex formazan yield of tryptophane and purity have been improved.In the whole reaction process, along with the adding of Inorganic Copper salts solution, the pH of reaction system is down to about 7 from 7.6-8.2 gradually; Thereby make a large amount of the separating out of tryptophane copper complex.
Beneficial effect
1. speed of reaction is significantly improved, and the reaction times is the shortest to be 0.5h;
2. than existing methods, the prepared copper complex formazan yield of tryptophane and the purity of preparation method of the present invention all is significantly improved; The copper complex formazan yield of tryptophane is more than 97.6%, and its purity is more than 98.8%;
3. the inorganic mantoquita that price is lower is excessive, the tryptophane complete reaction that price is higher; Save production cost;
4. step is simple, easy handling; Reacting balance.
Embodiment
Embodiment 1
The tryptophane of choosing 0.2 mole adds in 500 ml deionized water, adds sodium hydroxide, stirs, makes tryptophane to dissolve fully, and with pH modulation 7.6, then is heated to 80 ℃; 0.105 the mole cupric chloride adds the 80ml deionized water to fully dissolving.
Tryptophane solution is kept constant temperature; Under lasting agitation condition, Cupric Chloride Solution is added drop-wise in the tryptophane solution, the control rate of addition dropwises it in 0.5h; Then be cooled to 32 ℃.Reaction solution is taken out, carry out centrifugation; Then dry, pulverize, be packaged into finished product.Product yield is 97.64%, purity 98.87%.
Embodiment 2
The tryptophane of choosing 0.2 mole adds in 500 ml deionized water, and hydro-oxidation sodium stirs, makes tryptophane to dissolve fully, and pH is transferred to 7.9, then is heated to 89 ℃; 0.11 the mole cupric chloride adds the 70ml deionized water to fully dissolving.
Tryptophane solution is kept constant temperature; Continuing under the agitation condition, with the speed of 3ml/min Cupric Chloride Solution is being added drop-wise in the tryptophane solution; Change rate of addition into 1.5ml/min behind the 25min, dropwise behind the 17min; Then be cooled to 38 ℃.Reaction solution is taken out, carry out centrifugation; Then dry, pulverize, be packaged into finished product.Product yield is 97.71%, purity 99.06%.
Embodiment 3
The tryptophane of choosing 0.2 mole adds in 400 ml deionized water, and hydro-oxidation sodium stirs, makes tryptophane to dissolve fully, and pH is transferred to 8, then is heated to 96 ℃; 0.12 the mole cupric chloride adds the 40ml deionized water to fully dissolving.
Tryptophane solution is kept constant temperature; Continuing under the agitation condition, with the speed of 2ml/min Cupric Chloride Solution is being added drop-wise in the tryptophane solution; Change rate of addition into 0.5ml/min behind the 35min, dropwise behind the 20min; Then be cooled to 22 ℃.Reaction solution is taken out, carry out centrifugation; Then dry, pulverize, be packaged into finished product.Product yield is 98.29%, purity 99.19%.
Embodiment 4
The tryptophane of choosing 0.2 mole adds in 500 ml deionized water, and hydro-oxidation sodium stirs, makes tryptophane to dissolve fully, and pH is transferred to 8.2, then is heated to 99 ℃; 0.13 the mole cupric chloride adds the 40ml deionized water to fully dissolving.
Tryptophane solution is kept constant temperature; Continuing under the agitation condition, with the speed of 3.5ml/min Cupric Chloride Solution is being added drop-wise in the tryptophane solution; Change rate of addition into 1.5ml/min behind the 24min, dropwise behind the 10min; Then be cooled to 28 ℃.Reaction solution is taken out, carry out centrifugation; Then dry, pulverize, be packaged into finished product.Product yield is 97.94%, purity 98.97%.
Claims (6)
1. the copper complex formazan preparation method of fodder additives tryptophane is characterized in that, comprises the steps:
(1) according to the inorganic mantoquita of 1.05-1.3mol: the ratio of 2mol tryptophane is prepared raw material;
(2) with deionized water inorganic mantoquita is dissolved fully preparation Inorganic Copper salts solution;
(3) tryptophane is dissolved with sodium hydroxide solution, preparation pH is the tryptophane solution of 7.5-8.2;
(4) tryptophane solution is heated to 80-100 ℃, constant temperature continues to stir, and drips the Inorganic Copper salts solution to it, and 0.5-1h dropwises; Stir speed (S.S.) is 65-125r/min;
(5) be cooled to 20-40 ℃ after dropwising, then separate, drying, both product.
2. preparation method according to claim 1 is characterized in that, the mol ratio of described inorganic mantoquita and tryptophane is 1.1-1.2:2.
3. preparation method according to claim 1 is characterized in that, the temperature of described tryptophane solution is 85-95 ℃.
4. according to claim 1,2 or 3 described preparation methods, it is characterized in that the pH of described tryptophane solution is 7.9-8.
5. preparation method according to claim 4 is characterized in that, the rate of addition of the front 75-90% of Inorganic Copper salts solution is 2-4 times of afterwards rate of addition; Described percentage ratio is percent by volume.
6. preparation method according to claim 5 is characterized in that, stir speed (S.S.) is 65-85r/min.
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| CN2012105092852A CN102952060A (en) | 2012-12-04 | 2012-12-04 | Preparation method of feed additive tryptophane copper complex |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5071674A (en) * | 1973-11-01 | 1975-06-13 | ||
| US20090114602A1 (en) * | 2007-11-01 | 2009-05-07 | Logan Andrew J | Biosolids-based food additive for animal feed, methods of production, and business application thereof |
| CN101941938A (en) * | 2010-08-27 | 2011-01-12 | 长沙兴嘉生物工程股份有限公司 | Tryptophan chelate and preparation method and application thereof |
| CN102258123A (en) * | 2010-05-25 | 2011-11-30 | 陈士安 | Method for preparing feed additive-amino acid microelement chelate complex |
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2012
- 2012-12-04 CN CN2012105092852A patent/CN102952060A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5071674A (en) * | 1973-11-01 | 1975-06-13 | ||
| US20090114602A1 (en) * | 2007-11-01 | 2009-05-07 | Logan Andrew J | Biosolids-based food additive for animal feed, methods of production, and business application thereof |
| CN102258123A (en) * | 2010-05-25 | 2011-11-30 | 陈士安 | Method for preparing feed additive-amino acid microelement chelate complex |
| CN101941938A (en) * | 2010-08-27 | 2011-01-12 | 长沙兴嘉生物工程股份有限公司 | Tryptophan chelate and preparation method and application thereof |
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Application publication date: 20130306 |