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金属氨基磺酸盐的制备应该注意什么?
来源:http://www.jnjrh.com 日期:2019-08-14 发布人:admin
金属氨基磺酸盐,包括镍、钴、锡、铅、铜等数种金属的盐类,它们都是电镀主盐,因其有许多优点,如溶介度大(以氨基磺酸镍为例,它在水中的溶介度比硫酸镍大3.5倍),电镀产品内应力小(如用氨基磺酸镍电镀或电铸,其内应力只需硫酸镍的1/4),电镀或电铸速度特别快(用氨基磺酸镍电镀或电铸的速度比用硫酸镍快4倍),无环境污染等等,而被普遍地用在电镀或电铸工业中。但这些盐类的制造方法有的相当复杂,有的所用原料又相当昂贵,致使产质量量不是低劣,就是本钱过高,这些方法是1、碳酸镍法(苏联452543),以氨基磺酸分介碳酸镍制得,因消费碳酸镍时,需求参与多种化工原料,从而带入了大量杂质,影响了产品的质量。
Metal aminosulfonates, including salts of nickel, cobalt, tin, lead and copper, are the main salts for electroplating. They have many advantages, such as high solubility (taking nickel aminosulfonate as an example, its solubility in water is 3.5 times higher than that of nickel sulfate), and low internal stress (such as nickel aminosulfonate electroplating or electroforming) in electroplating products. Stress only needs 1/4 of nickel sulfate, and the electroplating or electroforming speed is very fast (the electroplating or electroforming speed with nickel sulfamate is four times faster than that with nickel sulfate). It has no environmental pollution and so on. It is widely used in electroplating or electroforming industry. However, some of these salts are quite complex, and some of the raw materials are quite expensive, resulting in either low quality or high cost. These methods are 1. Nickel carbonate process (USSR patent 452543), which is made from nickel carbonate separated by Aminosulfonic acid. When consuming nickel carbonate, it is necessary to participate in a variety of chemical raw materials. A lot of impurities are brought in, which affects the quality of the products.
、催化氧化法,这些方法分别用空气、氧气和过氧化氢在氨基磺酸溶液中,直接将粉状镍催化氧化制取氨基磺酸镍,该法的优点是工艺流程短,产质量量纯。但粉状镍价钱高,故产品本钱也高。
Catalytic oxidation method, which uses air, oxygen and hydrogen peroxide in Sulfamic Acid solution, directly oxidizes powdered nickel to produce nickel sulfamic acid. The advantage of this method is that the process is short and the yield is pure. But the price of powdered nickel is high, so the cost of the product is also high.
本发明抑制了上述两种方法的缺陷,采用了硫酸镍与氨基磺酸钡反响,以制取氨基磺酸镍,其反响为(1)由于硫酸钡溶介度极小,此法是一个快速不可逆反响,所得付产品也是一种常用的化工原料,将沉淀分别后,剩下的溶液便是所需求的产品了。
The invention restrains the defects of the above two methods, and adopts the reaction of nickel sulfate and barium sulfamate to produce nickel sulfamate. The reaction is (1) Because the solubility of barium sulfate is very small, this method is a fast and irreversible reaction, and the product is also a common chemical raw material. After precipitation, the remaining solution is convenient. It's the product you need.
按照相同的方法,以硫酸钴为原料可制取氨基磺酸钴(3)以硫酸亚锡为原料可制取氨基磺酸亚锡(4)以硫酸铜为原料也可制取氨基磺酸铜(5)等等。
According to the same method, cobalt sulfamate (3) can be prepared from cobalt sulfate, stannous sulfate (4) can be prepared from stannous sulfate, copper sulfamate (5) can be prepared from copper sulfate and so on.
本法的优点是消费流程简单,无环境污染,原料价廉,其消费本钱比任何方法都低,而产质量量与氧化法一样。
The advantages of this method are simple consumption process, no environmental pollution, low cost of raw materials, lower consumption cost than any other method, and the quality of production is the same as that of oxidation method.
例1、称取硫酸镍15.4克,溶于200毫升水中,再参与32.9克氨基磺酸钡,反响在搅拌下便疾速中止,待反响完成后,分别出沉淀硫酸钡,剩下的溶液就是氨基磺酸镍,蒸发烘干后可得32.2克Ni(NH2SO3)2·4H2O例2、称取氨基磺酸19.4克溶于200毫升水中,然后再缓缓参与19.7克碳酸钡,在搅拌下反响按下式疾速中止(2)待CO2全部放出后,参与15.4克硫酸镍(好是溶液)硫酸钡便立即沉淀出来,如例1将沉淀与溶液分别,蒸发烘干后也可得到32.2克Ni(NH2SO3)2·4H2O。上述两反响都是在常温下中止的。
Case 1: Nickel sulfate 15.4 grams, dissolved in 200 ml water, then participated in 32.9 grams of barium sulfamate. The reaction stopped rapidly under stirring. After the reaction was completed, barium sulfate was precipitated separately. The remaining solution was nickel sulfamate. After evaporation and drying, 32.2 grams of Ni (NH2SO3) 2.4H 2O case 2 was obtained. 19.4 grams of amino sulfonate was dissolved in 200. In milliliter water, then slowly participated in 19.7 grams of barium carbonate. Under stirring, the reaction stopped at a rapid click. (2) After all CO2 was released, barium sulfate participated in 15.4 grams of nickel sulfate (good solution) was precipitated immediately. For example, in case 1, precipitation was separated from solution. After evaporation and drying, 32.2 grams of Ni (NH2SO3) 2.4H 2O could also be obtained. Both of the above reactions stopped at room temperature.
例3、称取硫酸钴15.5克,溶于200毫升水中,再参与32.9克氨基磺酸钡,反响疾速中止,待反响完成后,分别出沉淀硫酸钡,剩下的溶液就是氨基磺酸钴,蒸发烘干后可得32.2克Co(NH2SO3)2·4H2O(注Ni与Co原子量相差无几)当然,也可称取与例2相同数量的氨基磺酸、碳酸钡以及硫酸钴,按同样的方法中止反响,所得结果相同。
氨基磺酸
Example 3: Take 15.5 grams of cobalt sulfate and dissolve in 200 ml water, then participate in 32.9 grams of barium sulfamate. The reaction stops rapidly. After the reaction is completed, barium sulfate is precipitated separately. The remaining solution is cobalt sulfamate. After evaporation and drying, 32.2 grams of Co (NH2SO3) 2.4H 2O can be obtained (the atomic weight of Ni and Co is almost the same). Of course, it is also desirable. The same amount of sulfamic acid, barium carbonate and cobalt sulfate as in Example 2 stopped the reaction in the same way, and the results were the same.
例4称取SnSO421.5克,溶于200毫升水中,再参与32.9克氨基磺酸钡,反响疾速中止,待反响完成后,分别出沉淀硫酸钡,剩下的溶液就是氨基磺酸亚锡,蒸发烘干后可得30克Sn(NH2SO3)2同样,也可按例2的方法,称取19.4克氨基磺酸和19.7克碳酸钡,在盛有200毫升的水中予先反响,生成氨基磺酸钡溶液,然后再参与21.5克的硫酸亚锡与之再反响,分别出硫酸钡沉淀,溶液也是Sn(NH2SO3)2例5称取CuSO416克,溶于200毫升水中,再参与32.9克氨基酸钡,反响疾速中止,待反响完成后,分别出沉淀硫酸钡,剩下的溶液便是氨基磺酸铜,蒸发烘干后可得Cu(NH2SO3)2·2H2O 29.8克。或者按例2方法反响,其结果一样。
Case 4 weighs SnSO421.5 g, dissolves in 200 ml water, then participates in 32.9 g of barium sulfamate. The reaction stops rapidly. After the reaction is completed, barium sulfate is precipitated separately. The remaining solution is stannous sulfamate. After evaporation and drying, 30 g of Sn (NH2SO3) 2 can be obtained. Similarly, 19.4 g of sulfamate and 19.7 g of barium sulfamate can also be obtained by case 2. Barium carbonate, which reacts first in 200 ml of water, forms barium sulfamate solution, then participates in 21.5 g of stannous sulfate and reacts with it. Barium Sulfate Precipitates separately. The solution is also Sn (NH2SO3) 2 cases, 5 cases, called CuSO416 g, dissolved in 200 ml of water, and then participates in 32.9 g of barium amino acid. The reaction rate stops and remains to be reacted. After the sound is finished, the precipitation of barium sulfate is separated. The remaining solution is copper aminosulfonate. After evaporation and drying, 29.8g of copper (NH2SO3) 2.2H 2O can be obtained. Or by example 2, the result is the same.
将溶介的硫酸镍参与到由(1)制备的氨基磺酸钡溶液中,在常温下,充分搅拌混合后,便生成了绿色的氨基磺酸镍,然后将溶液廓清分别出硫酸钡后,就得到所需求的产品氨基磺酸镍。上述两反响的特性是,在水溶液中中止,而且反响中止中要不时搅拌,在常温下就十分疾速。
The solution of nickel sulfate was added to the solution of barium sulfamate prepared by (1). At room temperature, after fully stirring and mixing, the green nickel sulfamate was formed. After the solution was cleared out and the barium sulfate was separated, the required product nickel sulfamate was obtained. The characteristics of the above two reactions are that they stop in aqueous solution and stir from time to time during the termination of the reactions, which is very rapid at room temperature.
由(1)制备的氨基磺酸钡,还可用于制取氨基酸钴,此时如(2)一样,将该盐的水溶液参与到氨基磺酸钡中,经搅拌反响,也能得到粉红色的氨基磺酸钴,其反响条件同(2)。
Barium sulfamate prepared from (1) can also be used to prepare cobalt amino acid. At this time, as (2), the aqueous solution of the salt is added to barium sulfamate, and pink cobalt sulfamate can also be obtained by stirring reaction. The reaction conditions are the same as (2).
同样如(2)将硫酸亚锡的溶液参与到氨基磺酸钡的溶液中,经搅拌反响也可得到乳白色的氨基磺酸亚锡。
Similarly, if (2) the solution of stannous sulfate is added to the solution of barium sulfamate, the milky white stannous sulfamate can be obtained by stirring reaction.
将硫酸铜溶介后,直接参与到由(1)制备的氨基磺酸钡中,经搅拌反响也可得到兰色的氨基磺酸铜。以上各反响的特征是,除了生成各种氨基磺酸盐外,还有付产品硫酸钡
After dissolving copper sulfate, it is directly involved in the preparation of barium sulfamate from (1). Blue copper sulfamate can also be obtained by stirring reaction. The above reactions are characterized by the formation of various sulfamate salts as well as barium sulfate as a paid product.