阅读说明：本技术 一种定性判定酸矿混合物酸解率程度的方法 (Method for qualitatively determining acidolysis rate degree of acid-ore mixture ) 是由 钱邦正 钱笑雄 李维健 钱林 于 2021-08-18 设计创作，主要内容包括：本发明公开了一种定性判定酸矿混合物酸解率程度的方法,包括以下步骤：(1)、取酸解结束的酸矿混合物20mL置于500mL锥形瓶中；(2)、加去离子水至200mL,煮沸5min；(3)、加水至500mL,充分摇匀,静置2min；(4)、倒去上层清夜300mL,再加水至500mL充分摇匀,静置2min,倒去300mL清夜,依次重复若干次得到待检验物；(5)、用不同酸解率的酸矿混合物作为标样,与待检验物比对沉淀物的量,以此确定待检验物的酸解率。本发明的有益效果是是提供一种简便、准确且时效性强的酸解率检测方法,能及时反馈生产做出相应调整酸矿混合物的酸解率,时效性强,操作简单,操作时间短。(The invention discloses a method for qualitatively determining the acidolysis rate degree of an acid-ore mixture, which comprises the following steps: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating the steps for several times to obtain a to-be-detected substance; (5) and comparing the amount of the precipitate with the amount of the to-be-detected object by using the acid ore mixture with different acidolysis rates as a standard sample, so as to determine the acidolysis rate of the to-be-detected object. The invention has the beneficial effects of providing a simple, convenient, accurate and strong-timeliness acidolysis rate detection method, being capable of feeding back production in time to correspondingly adjust the acidolysis rate of the acid ore mixture, being strong-timeliness, being simple to operate and being short in operation time.)

1. A method for qualitatively determining the acidolysis rate degree of an acid ore mixture is characterized by comprising the following steps: the method comprises the following steps: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating the steps for several times to obtain a to-be-detected substance; (5) and comparing the amount of the precipitate with the amount of the to-be-detected object by using the acid ore mixture with different acidolysis rates as a standard sample, so as to determine the acidolysis rate of the to-be-detected object.

2. The method for qualitatively determining the degree of acidolysis of an acid-ore mixture as claimed in claim 1, wherein: the acid ore mixture with different acidolysis rates comprises five acid ore mixtures with acidolysis rates of 90-91%, 92-93%, 94-95%, 96-97% and 98-99%, and the acidolysis degrees of the five acid ore mixtures are characterized as 2.5, 2.0, 1.5, 1.0 and 0.5.

Technical Field

The invention relates to the technical field of detection of acidolysis rate of ilmenite. In particular to a method for measuring the acidolysis rate of mixed titanium ore in the production process of titanium dioxide by a sulfuric acid method.

Background

In the prior art, most manufacturers in China adopt a sulfuric acid method to produce titanium dioxide, ilmenite is the most main raw material for producing titanium dioxide, and the utilization rate of the titanium dioxide resource by the production process can be directly mastered by the acidolysis rate of ilmenite in factories. Therefore, the acidolysis rate is an important index for controlling the production cost of the titanium white product, and the accuracy of the acidolysis rate plays an important guiding role in factory production and operation. In titanium white manufacturing enterprises, the method of measuring the acidolysis rate is generally to sample the leachate from the upper part of the acidolysis pot, filter and wash the leachate, and calculate the acidolysis rate by detecting the titanium content in the titanium solution and the residue, respectively.

Chinese patent publication No. CN102830200A discloses a method for detecting the acidolysis rate of a titanium-containing mineral, which comprises the following steps: analyzing chemical components of the titaniferous ore, and then determining the acid-ore ratio of acidolysis reaction; mixing a predetermined amount of titaniferous ore and concentrated sulfuric acid according to an acid-to-ore ratio to form a mixture; adding water into the mixture to dilute the concentrated sulfuric acid to 80-92% by mass; carrying out acidolysis reaction; after the acidolysis reaction is finished, curing to obtain a reaction product; leaching the reaction product under the condition of water bath; filtering, separating and leaching the obtained substance to obtain titanium liquid and residue, and calcining the residue; calculating the acidolysis rate according to formula 1, wherein formula 1 is: the acidolysis rate is mA/(mA + mB) × 100%.

For another example, chinese patent publication No. CN108414394A discloses a method for measuring the acidolysis rate of mixed titanium ore in the production process of titanium dioxide by a sulfuric acid process, comprising: detecting the grade of TiO2 of the ilmenite; adding concentrated sulfuric acid and ilmenite into an acidolysis pot, fully stirring, adding hydrolysis mother liquor, and diluting the concentrated sulfuric acid; after the acidolysis reaction is finished, obtaining a solid-phase substance, and after the solid-phase substance is cured, adding a leaching solution into an acidolysis pot to leach the acidolysis solid-phase substance; adding iron powder into an acidolysis pot for reduction reaction; sampling part of leaching solution in an acidolysis pot after reduction reaction is finished, carrying out suction filtration on the taken leaching solution to obtain titanium solution and residue, washing and drying the residue to constant weight, and detecting TiO in residue dry basis₂Grade of (d); measuring the total volume of the leaching solution obtained in the acidolysis pot after the reduction reaction is finished; and (4) calculating the acidolysis rate.

The measurement of the mixed titanium ore acidolysis rate in the above patents is quantitative measurement, and the acidolysis rate needs to be calculated, and although the method is accurate, the method consumes a great amount of time and is inconvenient to operate.

Disclosure of Invention

The invention aims to solve the technical problems that the existing method for measuring the acidolysis rate of titanium ore needs to wait for a long time, has poor timeliness, and provides a method for qualitatively determining the acidolysis rate degree of an acid-ore mixture.

The technical scheme of the invention is as follows: a method for qualitatively determining the acidolysis rate degree of an acid ore mixture comprises the following steps: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating the steps for several times to obtain a to-be-detected substance; (5) and comparing the amount of the precipitate with the amount of the to-be-detected object by using the acid ore mixture with different acidolysis rates as a standard sample, so as to determine the acidolysis rate of the to-be-detected object.

The acid mine mixtures with different acidolysis rates in the scheme comprise five acid mine mixtures with acidolysis rates of 90% -91%, 92% -93%, 94% -95%, 96% -97% and 98% -99%, and the acidolysis degrees of the five acid mine mixtures are defined as 2.5, 2.0, 1.5, 1.0 and 0.5.

The method has the advantages that the method is simple, convenient, accurate and strong in timeliness, calculation is not needed, the acidolysis rate of the acid ore mixture can be timely fed back to production to be correspondingly adjusted, timeliness is strong, operation is simple, and operation time is short.

Drawings

FIG. 1 is a photograph comparing an object to be examined with a standard sample having an acid-hydrolysis degree of 0.5 in the present invention;

FIG. 2 is a photograph comparing an object to be examined with a standard sample having an acid hydrolysis degree of qualitatively 1 according to the present invention;

FIG. 3 is a photograph comparing the specimen to be examined with a standard sample having an acid-hydrolysis degree of 1.5 in the present invention.

Detailed Description

The present invention will be further described with reference to the following examples.

Example 1: (1) taking 20mL of the acid ore mixture after the acid hydrolysis is finished, and placing the mixture into a 500mL conical flask; (2) adding deionized water to 200mL, and boiling for 5 min; (3) adding water to 500mL, shaking up fully, standing for 2 min; (4) pouring 300mL of supernatant, adding water to 500mL, fully shaking, standing for 2min, pouring 300mL of supernatant, and repeating for 4 times in sequence to obtain a to-be-detected substance; (5) the method comprises the steps of selecting five acid-ore mixtures with acidolysis rates of 90% -91%, 92% -93%, 94% -95%, 96% -97% and 98% -99% as standard samples, determining the acidolysis degrees of the five acid-ore mixtures to be 2.5, 2.0, 1.5, 1.0 and 0.5, comparing the amounts of black precipitates with an object to be detected, determining the range within which the acidolysis rate of the object to be detected falls, according to the requirement of target acidolysis rate, if the acidolysis rate of the object to be detected is lower than the target acidolysis rate, increasing the acidolysis rate of the acid-ore mixture where the object to be detected is located, and if the acidolysis rate of the object to be detected is higher than the target acidolysis rate, reducing the acidolysis rate of the acid-ore mixture where the object to be detected is located. As shown in FIG. 1, the test substance was found to be closest to the standard sample having an acid hydrolysis degree of 0.5 by comparison with five kinds of the standard samples, thereby determining the acid hydrolysis ratio of the test substance.

Example 2: the difference from example 1 is that the test substance was found to be closest to the standard sample of the acid hydrolysis degree 1 by comparing with five kinds of the standard samples as shown in FIG. 2, thereby determining the acid hydrolysis rate of the test substance.

Example 3: the difference from example 1 is that the acid hydrolysis rate of the specimen was determined by finding that it is closest to a standard sample having an acid hydrolysis degree of 1.5 by comparison with five standards as shown in FIG. 3.

The steps (1) to (4) of the invention are to add water or waste acid to extract the sampled ore pulp, remove the reacted titanium ore and finally precipitate the residual unreacted titanium slag, so that the result is closer to the actual value and the measurement is more accurate.