阅读说明：本技术 一种饲料级湿法磷酸深度净化方法 (Feed-grade wet-process phosphoric acid deep purification method ) 是由 陈海涛 王荣发 稂降龙 王勇 于 2020-11-19 设计创作，主要内容包括：本发明公开了一种饲料级湿法磷酸深度净化方法,包括以下步骤：步骤一：将改性无机盐、湿法磷酸、纯水按照比例混合,并进行搅拌,并静置沉淀；步骤二：将步骤一静置后的分层上部的液体去除,保留静置沉淀的残渣；步骤三：将步骤二中的残渣内加入硫酸,并通入氢氧化钠气体,得到矿物A；步骤四：将矿物A低温烘干,去除水份；步骤五：将步骤四中烘干的矿物A进行高温烘干,得到产品；通过添加的改性无机盐以及加工中的低温与高温的双重烘干,使得餐品内的因水份较大造成的结晶现象大幅度下降,极大的提高了成品的纯度,满足高质量的使用需求。(The invention discloses a feed-grade wet-process phosphoric acid deep purification method, which comprises the following steps: the method comprises the following steps: mixing the modified inorganic salt, wet-process phosphoric acid and pure water according to a proportion, stirring, and standing for precipitation; step two: removing the liquid on the upper part of the layer after standing in the step one, and reserving the residue of the standing precipitate; step three: adding sulfuric acid into the residue obtained in the step two, and introducing sodium hydroxide gas to obtain a mineral A; step four: drying the mineral A at low temperature, and removing water; step five: drying the mineral A dried in the fourth step at a high temperature to obtain a product; through the added modified inorganic salt and the dual drying of low temperature and high temperature in the processing, the crystallization phenomenon caused by large moisture in the meal is greatly reduced, the purity of the finished product is greatly improved, and the high-quality use requirement is met.)

1. A feed-grade wet-process phosphoric acid deep purification method is characterized by comprising the following steps: the method comprises the following steps:

the method comprises the following steps: mixing the modified inorganic salt, wet-process phosphoric acid and pure water according to a proportion, stirring, and standing for precipitation;

step two: removing the liquid on the upper part of the layer after standing in the step one, and reserving the residue of the standing precipitate;

step three: adding sulfuric acid into the residue obtained in the step two, and introducing sodium hydroxide gas to obtain a mineral A;

step four: drying the mineral A at low temperature, and removing water;

step five: and (4) drying the mineral A dried in the fourth step at a high temperature to obtain the product.

2. The feed-grade wet-process phosphoric acid deep purification method according to claim 1, characterized in that: the preparation method of the modified inorganic salt in the first step comprises the following steps:

step A: stirring and mixing sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide and sodium hydrogen phosphate according to a proportion, and continuously heating at a low temperature during stirring;

and B: b, drying the powder obtained in the step A at a high temperature, and placing the powder in a drying area;

and C: standing to obtain the modified inorganic salt.

3. The feed-grade wet-process phosphoric acid deep purification method according to claim 1, characterized in that: in the first step, the ratio of the modified inorganic salt to the wet-process phosphoric acid to the pure water is 1: 4: 5, stirring for 6-10 min, and standing for 4-7 h.

4. The feed-grade wet-process phosphoric acid deep purification method according to claim 1, characterized in that: and in the fourth step, the low-temperature drying temperature is 60-90 ℃, and the drying time is 30-50 min.

5. The feed-grade wet-process phosphoric acid deep purification method according to claim 1, characterized in that: and the high-temperature drying temperature in the fifth step is 400-600 ℃, and the drying time is 1-3 h.

6. The feed-grade wet-process phosphoric acid deep purification method according to claim 1, characterized in that: the low-temperature heating temperature in the step A is 70-90 ℃, and the ratio of sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide to sodium hydrogen phosphate is 1: 1: 1: 2: 1: 2.

7. the feed-grade wet-process phosphoric acid deep purification method according to claim 1, characterized in that: and the high-temperature drying temperature in the step B is 300-500 ℃.

Technical Field

The invention belongs to the technical field of wet-process phosphoric acid, and particularly relates to a feed-grade wet-process phosphoric acid deep purification method.

Background

The wet-process phosphoric acid refers to the phosphoric acid obtained by decomposing phosphate ore with sulfuric acid, nitric acid or hydrochloric acid, which is collectively called wet-process phosphoric acid, and the method for decomposing phosphate ore with sulfuric acid is the most basic method in the production of wet-process phosphoric acid, and at present, the production methods of phosphoric acid mainly comprise a thermal method and a wet method. The phosphoric acid by a thermal method is used for preparing yellow phosphorus by an electric furnace method, and pure industrial phosphoric acid is obtained by oxidation and absorption; the wet-process phosphoric acid is used for decomposing phosphorite by strong acid such as sulfuric acid or hydrochloric acid.

In practical application, the existing wet-process phosphoric acid deep purification method has an unobvious impurity removal effect, high-purity phosphoric acid cannot be obtained, phosphoric acid containing various impurities is obtained after liquid-solid separation, and wet-process phosphoric acid is generally used for preparing phosphate fertilizers and needs to be further purified if high-quality phosphate products are prepared.

Disclosure of Invention

The invention aims to provide a feed-grade wet-process phosphoric acid deep purification method to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a feed-grade wet-process phosphoric acid deep purification method comprises the following steps:

the method comprises the following steps: mixing the modified inorganic salt, wet-process phosphoric acid and pure water according to a proportion, stirring, and standing for precipitation;

step two: removing the liquid on the upper part of the layer after standing in the step one, and reserving the residue of the standing precipitate;

step three: adding sulfuric acid into the residue obtained in the step two, and introducing sodium hydroxide gas to obtain a mineral A;

step four: drying the mineral A at low temperature, and removing water;

step five: and (4) drying the mineral A dried in the fourth step at a high temperature to obtain the product.

Preferably, the preparation of the modified inorganic salt in the step one comprises the following steps:

step A: stirring and mixing sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide and sodium hydrogen phosphate according to a proportion, and continuously heating at a low temperature during stirring;

and B: b, drying the powder obtained in the step A at a high temperature, and placing the powder in a drying area;

and C: standing to obtain the modified inorganic salt.

Preferably, the ratio of the modified inorganic salt, the wet-process phosphoric acid and the pure water in the first step is 1: 4: 5, stirring for 6-10 min, and standing for 4-7 h.

Preferably, the low-temperature drying temperature in the fourth step is 60-90 ℃, and the drying time is 30-50 min.

Preferably, the high-temperature drying temperature in the fifth step is 400-600 ℃, and the drying time is 1-3 hours.

Preferably, the low-temperature heating temperature in the step A is 70-90 ℃, and the ratio of sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide and sodium hydrogen phosphate is 1: 1: 1: 2: 1: 2.

preferably, the high-temperature drying temperature in the step B is 300-500 ℃.

Compared with the prior art, the invention has the beneficial effects that:

through the added modified inorganic salt and the dual drying of low temperature and high temperature in the processing, the crystallization phenomenon caused by large moisture in the meal is greatly reduced, the purity of the finished product is greatly improved, and the high-quality use requirement is met.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The invention provides a technical scheme that: a feed-grade wet-process phosphoric acid deep purification method comprises the following steps:

the method comprises the following steps: mixing the modified inorganic salt, wet-process phosphoric acid and pure water according to a proportion, stirring, and standing for precipitation;

step two: removing the liquid on the upper part of the layer after standing in the step one, and reserving the residue of the standing precipitate;

step three: adding sulfuric acid into the residue obtained in the step two, and introducing sodium hydroxide gas to obtain a mineral A;

step four: drying the mineral A at low temperature, and removing water;

step five: and (4) drying the mineral A dried in the fourth step at a high temperature to obtain the product.

In this embodiment, preferably, the preparation of the modified inorganic salt in the step one comprises the following steps:

step A: stirring and mixing sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide and sodium hydrogen phosphate according to a proportion, and continuously heating at a low temperature during stirring;

and B: b, drying the powder obtained in the step A at a high temperature, and placing the powder in a drying area;

and C: standing to obtain the modified inorganic salt.

In this embodiment, preferably, the ratio of the modified inorganic salt, the wet-process phosphoric acid and the pure water in the step one is 1: 4: 5, stirring time is 10min, and standing time is 7 h.

In this embodiment, preferably, the low-temperature drying temperature in the fourth step is 90 ℃, and the drying time is 50 min.

In this embodiment, preferably, the high-temperature drying temperature in the fifth step is 600 ℃, and the drying time is 3 hours.

In this embodiment, preferably, the low-temperature heating temperature in step a is 90 ℃, and the ratio of sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide, and sodium hydrogen phosphate is 1: 1: 1: 2: 1: 2.

in this embodiment, preferably, the high-temperature drying temperature in step B is 500 ℃.

Example 2

The invention provides a technical scheme that: a feed-grade wet-process phosphoric acid deep purification method comprises the following steps:

the method comprises the following steps: mixing the modified inorganic salt, wet-process phosphoric acid and pure water according to a proportion, stirring, and standing for precipitation;

step two: removing the liquid on the upper part of the layer after standing in the step one, and reserving the residue of the standing precipitate;

step three: adding sulfuric acid into the residue obtained in the step two, and introducing sodium hydroxide gas to obtain a mineral A;

step four: drying the mineral A at low temperature, and removing water;

step five: and (4) drying the mineral A dried in the fourth step at a high temperature to obtain the product.

In this embodiment, preferably, the preparation of the modified inorganic salt in the step one comprises the following steps:

step A: stirring and mixing sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide and sodium hydrogen phosphate according to a proportion, and continuously heating at a low temperature during stirring;

and B: b, drying the powder obtained in the step A at a high temperature, and placing the powder in a drying area;

and C: standing to obtain the modified inorganic salt.

In this embodiment, preferably, the ratio of the modified inorganic salt, the wet-process phosphoric acid and the pure water in the step one is 1: 4: 5, stirring for 8min and standing for 5 h.

In this embodiment, preferably, the low-temperature drying temperature in the fourth step is 80 ℃, and the drying time is 40 min.

In this embodiment, preferably, the high-temperature drying temperature in the fifth step is 500 ℃, and the drying time is 2 hours.

In this embodiment, preferably, the low-temperature heating temperature in step a is 80 ℃, and the ratio of sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide, and sodium hydrogen phosphate is 1: 1: 1: 2: 1: 2.

in this embodiment, preferably, the high-temperature drying temperature in step B is 400 ℃.

Example 3

The invention provides a technical scheme that: a feed-grade wet-process phosphoric acid deep purification method comprises the following steps:

the method comprises the following steps: mixing the modified inorganic salt, wet-process phosphoric acid and pure water according to a proportion, stirring, and standing for precipitation;

step two: removing the liquid on the upper part of the layer after standing in the step one, and reserving the residue of the standing precipitate;

step three: adding sulfuric acid into the residue obtained in the step two, and introducing sodium hydroxide gas to obtain a mineral A;

step four: drying the mineral A at low temperature, and removing water;

step five: and (4) drying the mineral A dried in the fourth step at a high temperature to obtain the product.

In this embodiment, preferably, the preparation of the modified inorganic salt in the step one comprises the following steps:

step A: stirring and mixing sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide and sodium hydrogen phosphate according to a proportion, and continuously heating at a low temperature during stirring;

and B: b, drying the powder obtained in the step A at a high temperature, and placing the powder in a drying area;

and C: standing to obtain the modified inorganic salt.

In this embodiment, preferably, the ratio of the modified inorganic salt, the wet-process phosphoric acid and the pure water in the step one is 1: 4: 5, stirring time is 6min, and standing time is 4 h.

In this embodiment, preferably, the low-temperature drying temperature in the fourth step is 60 ℃, and the drying time is 30 min.

In this embodiment, preferably, the high-temperature drying temperature in the fifth step is 400 ℃, and the drying time is 1 h.

In this embodiment, preferably, the low-temperature heating temperature in step a is 70 ℃, and the ratio of sodium carbonate, potassium carbonate, magnesium carbonate, ammonium carbonate, sodium hydroxide, and sodium hydrogen phosphate is 1: 1: 1: 2: 1: 2.

in this embodiment, preferably, the high-temperature drying temperature in step B is 300 ℃.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.