Preparation method of basic copper acetate

Abstract

The invention discloses a preparation method of basic copper acetate, which comprises the following steps: mixing an acetic acid solution with an alkaline copper source, heating for reaction to obtain a solid-liquid mixture of basic copper acetate, centrifuging to obtain a centrifugal mother solution and a solid phase, and drying the solid phase to obtain the basic copper acetate. According to the preparation method of the basic copper acetate, the basic copper source and the acetic acid solution are used for heating reaction, the reaction liquid obtained after the reaction is completed is subjected to centrifugal separation, washing and drying in the drying device to obtain the basic copper acetate product, and the process is simple in production, complete in copper oxide reaction, few in by-products, capable of recycling centrifugal mother liquor, free of environmental pollution and environmentally friendly; the cost is low. The preparation method is beneficial to large-scale industrial production of basic copper acetate and can be widely applied to the field of animal feed additives.

Description

Technical Field

[0001] The invention belongs to the field of feed additives, and in particular relates to a method for preparing a copper-containing additive. Background Art

[0002] The content of copper in organisms is very small, but its role is very huge: copper can promote the normal function of blood, central nervous system and immune system; copper is involved in the synthesis of various enzymes (such as tyrosinase, monoamine oxidase, superoxidase, etc.), and can effectively participate in the body's cell oxidation, bone and connective tissue formation, keratinization and tissue pigmentation; copper can also maintain the normal bones, blood vessels and skin, and plays an important role in maintaining normal heart function; copper can also promote iron absorption and function, maintain normal iron metabolism, and is beneficial to hemoglobin synthesis and red blood cell maturation; copper also plays a very important role in improving the quality of poultry eggshells. In addition to supplementing the trace element copper, copper acetate also has a unique effect on controlling Salmonella in broiler farming.

[0003] Basic copper acetate is a good copper supplement. Currently, basic copper acetate on the market is mainly obtained by the reaction of copper acetate and sodium hydroxide. The reaction produces sodium acetate as a by-product, and the recovery and treatment of the by-product is difficult and costly. Summary of the invention

[0004] The technical problem to be solved by the present invention is to overcome the deficiencies and defects mentioned in the above background technology and provide a method for preparing basic copper acetate with less by-products and green environmental protection.

[0005] In order to solve the above technical problems, the technical solution proposed by the present invention is: A method for preparing basic copper acetate comprises the following steps: mixing an acetic acid solution with an alkaline copper source, heating for reaction to obtain a solid-liquid mixture of basic copper acetate, centrifuging to obtain a centrifugal mother liquor and a solid phase, and drying the solid phase to obtain the basic copper acetate.

[0006] In the above preparation method, preferably, the alkaline copper source is copper oxide and / or copper hydroxide.

[0007] In the present invention, our research shows that acetic acid is a medium-strong acid with strong acidity, and the copper source is an alkaline oxide, which is easy to react with acetic acid, but the reaction conditions need to be controlled so that the reaction product is basic copper acetate, rather than copper acetate. The difficulty in controlling the reaction conditions lies in the ratio of acetic acid and the alkaline copper source and the concentration at which the reaction is carried out so that the reaction product is not wrapped on the alkaline copper source, and the copper source reacts completely to obtain the target product.

[0008] In the above preparation method, preferably, the molar ratio of the alkaline copper source to acetic acid is 1: (0.5-1). More preferably, the molar ratio of the alkaline copper source to acetic acid is 1: (0.5-0.7). The molar ratio of the alkaline copper source to acetic acid will determine the type and purity of the reaction product. If it is not controlled within the above range, either unreacted copper source will be present in the product, or copper acetate will be obtained instead of basic copper acetate. Therefore, the above molar ratio needs to be precisely controlled.

[0009] In the above preparation method, preferably, the acetic acid solution is a solution of glacial acetic acid diluted with water or centrifuged mother liquor, and the mass concentration of the acetic acid solution is 20-70%. More preferably, the mass concentration of the acetic acid solution is 40-60%. The mass concentration of the above acetic acid solution is also the key to determining the type and purity of the reaction product. If the concentration is not controlled within the above range, the reaction product will be wrapped on the raw copper source if the concentration is too high, and the production efficiency is low and the energy consumption cost is high if the concentration is too low.

[0010] In the above preparation method, preferably, the fineness of the alkaline copper source is less than 50 um. The fineness of the alkaline copper source will also affect the type and purity of the reaction product, and its fineness should not be too large, otherwise it will lead to a decrease in the purity of the reaction product, basic copper acetate.

[0011] In the above preparation method, preferably, the heating reaction is carried out in an enameled reactor.

[0012] In the above preparation method, preferably, when heating the reaction, the reaction temperature is controlled to be 70-120°C and the reaction time is 1-6h. More preferably, the reaction temperature is controlled to be 80-100°C and the reaction time is 2-4h. If the temperature is too low, the reaction speed is too slow and the reaction is incomplete. If the temperature is too high, the energy consumption is high and the acetic acid volatilization loss is large. If the time is too short, the reaction is incomplete.

[0013] In the above preparation method, preferably, air flow drying is adopted during solid phase drying, and the drying equipment includes a flash fast dryer or a straight tube air flow dryer.

[0014] The preparation method of basic copper acetate of the present invention, more specifically, comprises the following steps: (1) Add glacial acetic acid into an enameled reactor, stir, add water or centrifuge the mother liquor to prepare an acetic acid solution of a certain concentration; (2) Adding alkaline copper source into the enamel reactor according to the formula ratio; (3) Start the steam heating reaction to obtain a solid-liquid mixture of basic copper acetate; (4) Centrifugation to obtain a centrifugal mother liquor and a solid phase, and the centrifugal mother liquor is recycled; (5) Solid phase drying yields basic copper acetate product.

[0015] The present invention uses a copper source and acetic acid as raw materials to react under heating conditions to prepare basic copper acetate (Cu2(OH)3CH3COO)·H2O, and the chemical reaction equation is as follows: 2CuO+CH3COOH+2H2O→Cu2(OH)3CH3COO)·H2O; 2Cu(OH)2+CH3COOH→Cu2(OH)3CH3COO)·H2O.

[0016] Compared with the prior art, the advantages of the present invention are: The preparation method of basic copper acetate of the present invention utilizes an alkaline copper source and an acetic acid solution for heating reaction, and the reaction liquid after the reaction is completed is centrifuged, washed, and then dried in a drying device to obtain a basic copper acetate product. The process is simple to produce, the copper oxide reaction is complete, there are few by-products, the centrifuged mother liquor can be recycled, there is no environmental pollution, it is green and environmentally friendly, and the cost is low. The above-mentioned preparation method is conducive to the large-scale industrial production of basic copper acetate, and can be widely used in the field of animal feed additives. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1 The present invention is a process flow chart of the preparation method of basic copper acetate. DETAILED DESCRIPTION

[0019] In order to facilitate the understanding of the present invention, the present invention will be described more comprehensively and meticulously below in conjunction with the accompanying drawings and preferred embodiments of the present invention, but the protection scope of the present invention is not limited to the following specific embodiments.

[0020] Unless otherwise defined, all the professional terms used below have the same meanings as those generally understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention.

[0021] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

[0022] Embodiment 1: like Figure 1 As shown, a method for preparing basic copper acetate comprises the following steps: Add 360kg of glacial acetic acid and 360kg of tap water into 2m 3 In an enameled reactor (prepared with 50% acetic acid solution), stir, add 980kg of copper oxide with a fineness less than 50um (copper source: acetic acid is about 1:0.5, molar ratio, the same below), heat to 85℃, and react at constant temperature for 180 minutes. After the reaction is completed, centrifuge with a bag centrifuge, wash with a small amount of water, and flash dry at 100℃ to obtain the product. After testing, the copper content in the product is 48.5%, the acetate content is 22.7%, the purity of basic copper acetate is 97.0%, the product also contains 1% free acetic acid, 2% water, and the product is a green crystalline substance.

[0023] Embodiment 2: like Figure 1 As shown, a method for preparing basic copper acetate comprises the following steps: Add 380 kg of glacial acetic acid, 340 kg of the mother liquor from Example 1, and 200 kg of tap water into a 2 m 3 In an enameled reactor (prepared with 41% acetic acid solution), stir, add 900kg of copper oxide with a fineness of less than 50um (copper source: acetic acid is about 1:0.57), heat to 90℃, and react at constant temperature for 150 minutes. After the reaction is completed, centrifuge, wash with a small amount of water, and flash dry at 100℃ to obtain the product. After testing, the copper content in the product is 48.4%, the acetate content is 22.6%, the purity of basic copper acetate is 96.8%, the product also contains 1% free acetic acid, about 0.13% copper oxide, and 2.07% water. The product is a green crystalline substance.

[0024] Embodiment 3: like Figure 1 As shown, a method for preparing basic copper acetate comprises the following steps: Add 400kg of glacial acetic acid and 300kg of tap water into a 2m 3 In an enameled reactor (prepared with 57% acetic acid solution), stir, add 1250kg of copper hydroxide with a fineness of less than 50um (copper source: acetic acid is about 1:0.54), heat to 95℃, and react at constant temperature for 120 minutes. After the reaction is completed, centrifuge, wash with a small amount of water, and flash dry at 100℃ to obtain the product. After testing, the copper content in the product is 48.9%, the acetate content is 22.8%, the purity of basic copper acetate is 97.8%, the product also contains 1.2% free acetic acid, about 0.65% copper oxide, and 0.35% water. The product is a green crystalline substance.

[0025] Embodiment 4: like Figure 1 As shown, a method for preparing basic copper acetate comprises the following steps: Add 400kg of glacial acetic acid and 400kg of tap water into a 2m3 In an enameled reactor (prepared with 50% acetic acid solution), stir, add 1000kg of copper hydroxide with a fineness of less than 50um (copper source: acetic acid is about 1:0.68), heat to 100℃, react at constant temperature for 150 minutes. After the reaction is completed, centrifuge, wash with a small amount of water, and flash dry at 100℃ to obtain the product. After testing, the copper content in the product is 49.0%, the acetate content is 22.8%, the purity of basic copper acetate is 97.8%, the product also contains 1.2% free acetic acid, about 0.79% copper oxide, and 0.2% water. The product is a green crystalline substance.

[0026] Embodiment 5: like Figure 1 As shown, a method for preparing basic copper acetate comprises the following steps: Add 360kg of glacial acetic acid and 360kg of tap water into 2m 3 In an enameled reactor (prepared with 50% acetic acid solution), stir, add 625kg of copper hydroxide with a fineness of less than 50um (copper source: acetic acid is about 1:0.96), heat to 85℃, and react at constant temperature for 240 minutes. After the reaction is completed, centrifuge, wash with a small amount of water, and dry in a 100℃ air flow to obtain the product. After testing, the copper content in the product is 48.0%, the acetate content is 22.3%, the purity of basic copper acetate is 96%, the product also contains 0.7% free acetic acid, 3.3% water, and the product is a green crystalline substance.

[0027] Comparative Example 1: A method for preparing basic copper acetate comprises the following steps: Add 380kg of glacial acetic acid and 150kg of tap water into a 2m 3 In an enameled reactor (prepared with 72% acetic acid solution), stir, add 1325kg of copper oxide with a fineness of less than 50um (copper source: acetic acid is about 1:0.4), heat to 90℃, and react at constant temperature for 150 minutes. After the reaction is completed, centrifuge, wash with a small amount of water, and flash dry at 100℃ to obtain the product. After testing, the copper content in the product is 57.1%, the acetate content is 18.3%, the purity of basic copper acetate is 69.4%, and the product is a black powder.

Claims

1. A method for preparing basic copper acetate, characterized in that: The following steps are involved: The acetic acid solution is mixed with an alkaline copper source, heated for reaction, and a solid-liquid mixture of basic copper acetate is obtained. The mixture is centrifuged to obtain a centrifugal mother liquor and a solid phase, and the solid phase is dried to obtain the basic copper acetate.

2. The preparation method according to claim 1, characterized in that: The alkaline copper source is copper oxide and / or copper hydroxide.

3. The preparation method according to claim 1, characterized in that: The molar ratio of the alkaline copper source to acetic acid is 1:(0.5-1).

4. The preparation method according to claim 3, characterized in that: The molar ratio of the alkaline copper source to acetic acid is 1:(0.5-0.7).

5. The preparation method according to claim 1, characterized in that: The acetic acid solution is a solution obtained by diluting glacial acetic acid with water or centrifuged mother liquor, and the mass concentration of the acetic acid solution is 20-70%.

6. The preparation method according to claim 5, characterized in that: The mass concentration of the acetic acid solution is 40-60%.

7. The preparation method according to claim 1, characterized in that: The fineness of the alkaline copper source is less than 50 um.

8. The preparation method according to claim 1, characterized in that: When heating the reaction, the reaction temperature is controlled to be 70-120°C and the reaction time is 1-6h.

9. The preparation method according to claim 8, characterized in that: The reaction temperature was controlled at 80-100°C and the reaction time was 2-4h.

10. The preparation method according to claim 1, characterized in that: Air flow drying is used for solid phase drying, and the drying equipment includes a flash quick dryer or a straight tube air flow dryer.

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