A kind of preparation process of high-purity sulfuric acid barium

文档序号:1765745 发布日期:2019-12-03 浏览:33次 中文

阅读说明:本技术 一种高纯度硫酸钡的制备工艺 (A kind of preparation process of high-purity sulfuric acid barium ) 是由 徐顺保 赵志鹏 于 2019-08-28 设计创作,主要内容包括:本发明涉及硫酸钡技术领域,尤其是一种高纯度硫酸钡的制备工艺,包括以下步骤:S1、制备稀硫酸溶液;S2、对氯化钡溶液与稀硫酸溶液进行称重;S3、对反应制得的溶液进行过滤,将沉淀物进行取出,进行水洗,水洗的温度为50-60℃,清洗次数为3-5次,并对清洗所的溶液中的钡离子检测,然后对其进过滤取出沉淀物,在温度为80-90℃环境中对沉淀物进行干燥,时间为8-12h,在干燥的过程中;S4、将过滤后所得到的溶液为盐酸,加入碳酸钡粉末,在加入时进行搅拌,在温度为2-5℃的环境中静置30-45min;S5、将S4反应制得的溶液与再与稀硫酸溶液进行反应。本发明具有提高了硫酸钡的纯度,同时对溶液进行重复利用避免了产生的废液造成污染。(The present invention relates to barium sulfate technical field, especially a kind of preparation process of high-purity sulfuric acid barium, comprising the following steps: S1, prepare dilution heat of sulfuric acid;S2, it weighs to barium chloride solution and dilution heat of sulfuric acid;S3, reaction solution obtained is filtered, sediment is taken out, it is washed, the temperature of washing be 50-60 DEG C, wash number be 3-5 time, and to cleaning solution in barium ions detection, then sediment is taken out into filtering to it, it is that sediment is dried in 80-90 DEG C of environment in temperature, time 8-12h, during drying;S4, it will obtained solution be hydrochloric acid after filtering, barium carbonate powder is added, is stirred when being added, is to stand 30-45min in 2-5 DEG C of environment in temperature;S5, S4 is reacted solution obtained with reacted again with dilution heat of sulfuric acid.The present invention, which has, improves the purity of barium sulfate, while carrying out recycling to solution and avoid the waste liquid of generation polluting.)

1. a kind of preparation process of high-purity sulfuric acid barium, which comprises the following steps:

S1, dilution heat of sulfuric acid is prepared, dilution heat of sulfuric acid is directly diluted with the concentrated sulfuric acid;

S2, it weighs to barium chloride solution and dilution heat of sulfuric acid, and molal weight ratio is 1:1, dilution heat of sulfuric acid is slow It is poured into barium chloride solution, and is stirred using glass bar, stand 30-60min;

S3, reaction solution obtained is filtered, sediment is taken out, is washed, the temperature of washing is 50-60 DEG C, wash number be 3-5 time, and to cleaning institute solution in barium ions detect, then to its into filter taking-up sediment, In Temperature is that sediment is dried in 80-90 DEG C of environment, time 8-12h, is carried out during drying, and to sediment Stirring, after drying, and grinds sediment;

It S4, is hydrochloric acid by obtained solution after filtering, addition barium carbonate powder is stirred when being added, and is 2-5 in temperature DEG C environment in stand 30-45min, observe in solution whether there are also white depositions, if there is continuously adding hydrochloric acid solution, directly It is dissolved to precipitating;

S5, S4 is reacted solution obtained with reacted again with dilution heat of sulfuric acid.

2. a kind of preparation process of high-purity sulfuric acid barium according to claim 1, which is characterized in that carry out in step s3 When barium ions detects, comprising the following steps:

A1, it resulting solution will be cleaned continuously adds a small amount of dilution heat of sulfuric acid, and be stirred;

When A2, standing 10-15min, whether the bottom for observing solution has white precipitate;

A3, there is white precipitate to be taken out sediment, and cleaning acquired solution is mixed with filtered fluid.

3. a kind of preparation process of high-purity sulfuric acid barium according to claim 1, which is characterized in that carrying out, dilute sulfuric acid is molten When liquid is produced, is weighed, the concentrated sulfuric acid is added slowly in water, and it is stirred to water and the concentrated sulfuric acid by calculating It mixes, it is ensured that even heat when concentrated sulfuric acid dissolution sheds.

4. a kind of preparation process of high-purity sulfuric acid barium according to claim 1, which is characterized in that carried out to sediment When grinding, comprising the following steps:

B1, sediment is screened first, the sediment of bulk is crushed;

B2, broken sediment is tentatively crushed, crushed material is screened using 80 meshes, it will be complete without crushing It is tentatively crushed again;

B3, the carry out separating twice for crushing B2, screen crushed material using 400 meshes, will be not over 400 meshes Carry out separating twice again.

5. a kind of preparation process of high-purity sulfuric acid barium according to claim 1, which is characterized in that the barium carbonate powder Molal weight ratio with hydrochloric acid is 1:2.

6. a kind of preparation process of high-purity sulfuric acid barium according to claim 1, which is characterized in that the dilute sulfuric acid uses It is prepared by the concentrated sulfuric acid that concentration is 98%.

Technical field

The present invention relates to barium sulfate technical field more particularly to a kind of preparation processes of high-purity sulfuric acid barium.

Background technique

The mineral products of barium sulfate are called barite.For white amorphous powder.Property is stablized, and water, acid, alkali or organic are insoluble in Solvent.Radiological examination mainly can absorb X-ray in gastrointestinal tract using it using barium sulfate agent and acts on its development, therefore It is mainly used as gastrointestinal tract contrast medium.When being produced to barium sulfate, using barite ore to purification to barium sulfate system It takes, but when being produced, a large amount of impurity can be contained in ore, shadow can be generated to the purity of the barium sulfate prepared It rings, so it is proposed that a kind of preparation process of high-purity sulfuric acid barium.

Summary of the invention

The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of high-purity sulfuric acid barium proposed Preparation process.

To achieve the goals above, present invention employs following technical solutions:

Design a kind of preparation process of high-purity sulfuric acid barium, comprising the following steps:

S1, dilution heat of sulfuric acid is prepared, dilution heat of sulfuric acid is directly diluted with the concentrated sulfuric acid;

S2, it weighs to barium chloride solution and dilution heat of sulfuric acid, and molal weight ratio is 1:1, and dilution heat of sulfuric acid is delayed Slow is poured into barium chloride solution, and is stirred using glass bar, stands 30-60min;

S3, reaction solution obtained is filtered, sediment is taken out, is washed, the temperature of washing is 50- 60 DEG C, wash number be 3-5 time, and to cleaning institute solution in barium ions detect, then to its into filter taking-up sediment, Temperature be 80-90 DEG C of environment in sediment is dried, time 8-12h, during drying, and to sediment into Row stirring, after drying, and grinds sediment;

It S4, is hydrochloric acid by obtained solution after filtering, addition barium carbonate powder is stirred, in temperature when being added To stand 30-45min in 2-5 DEG C of environment, observe in solution whether there are also white depositions, it is molten if there is continuously adding hydrochloric acid Liquid, until precipitating dissolution;

S5, S4 is reacted solution obtained with reacted again with dilution heat of sulfuric acid.

Preferably, when carrying out barium ions detection in step s3, comprising the following steps:

A1, it resulting solution will be cleaned continuously adds a small amount of dilution heat of sulfuric acid, and be stirred;

When A2, standing 10-15min, whether the bottom for observing solution has white precipitate;

A3, there is white precipitate to be taken out sediment, and cleaning acquired solution is mixed with filtered fluid.

Preferably, it when progress dilution heat of sulfuric acid is produced, is weighed by calculating to water and the concentrated sulfuric acid, the concentrated sulfuric acid is delayed Slow is added to the water, and is stirred to it, it is ensured that even heat when concentrated sulfuric acid dissolution sheds.

Preferably, when being ground to sediment, comprising the following steps:

B1, sediment is screened first, the sediment of bulk is crushed;

B2, broken sediment is tentatively crushed, crushed material is screened using 80 meshes, it will be without having crushed Complete is tentatively crushed again;

B3, the carry out separating twice for crushing B2, screen crushed material using 400 meshes, will be not over 400 The carry out separating twice again of mesh.

Preferably, the molal weight of the barium carbonate powder and hydrochloric acid ratio is 1:2.

Preferably, the dilute sulfuric acid uses concentration to prepare for 98% concentrated sulfuric acid.

A kind of preparation process of high-purity sulfuric acid barium proposed by the present invention, beneficial effect are: the introducing of impurity is avoided, To improve the purity for preparing barium sulfate, while preparation method is easy to operate, and the solution generated to reaction carries out weight It is multiple to utilize, cost is saved, while the waste liquid for also avoiding generating pollutes, while during preparation, not generating Pernicious gas and dangerous goods increase safety when preparation.

Specific embodiment

Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.

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