CN107793446A - A kind of purification process of SILVER REAGENT tributyl phosphate - Google Patents

Abstract

The invention provides a kind of purification process of SILVER REAGENT tributyl phosphate, comprise the following steps that：(1) 1.2 1.5% nitric acid are added into tributyl phosphate and are stirred, liquid separation removes nitric acid layer；(2) continuously washed with 0.6 0.8% sodium hydroxide solution again, each sodium hydroxide discards, then not aobvious alkaline with pure water to water layer PH；(3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤0.08MPa, discards front-end volatiles, produce；Methods described technique is simple, and product purity is high, and operating condition is gentle, is adapted to the needs of scale industrial production.

Description

A kind of purification process of SILVER REAGENT tributyl phosphate

Technical field

The present invention relates to a kind of method of purification of chemical reagent, especially a kind of purifying side of SILVER REAGENT tributyl phosphate Method.

Background technology

Tributyl phosphate, cas126-73-8, as GC stationary liquid, extraction cobalt, iridium, manganese, molybdenum, palladium, rhodium, nickel, uranium And tungsten, colorimetric estimation molybdenum.Can also be used for the solvent of nitrocellulose and ethyl cellulose, plasticizer, rare earth metal separation agent and Organic synthesis intermediate.

Tributyl phosphate, major impurity is organic pyrophosphate, only son's based phosphates, dibutylphosphoric acid in industrial products Salt, butanol etc., product quality do not meet reagent standard, need to be purified applied to reagent.

The content of the invention

The technical problems to be solved by the invention are to provide a kind of purification process of SILVER REAGENT tributyl phosphate.

In order to solve the above technical problems, the technical scheme is that：

A kind of purification process of SILVER REAGENT tributyl phosphate, specific preparation process are as follows：

(1) 1.2-1.5% nitric acid is added into tributyl phosphate and is stirred, liquid separation removes nitric acid layer；

(2) continuously washed with 0.6-0.8% sodium hydroxide solution again, each sodium hydroxide discards, then is washed with pure water Wash to the not aobvious alkalescence of water layer PH；

(3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤- 0.08MPa, discards front-end volatiles, produce.

Preferably, the purification process of mentioned reagent level tributyl phosphate, the tributyl phosphate and 1.2-1.5% nitric acid Volume ratio is 10:1.

The beneficial effects of the invention are as follows：

The purification process of mentioned reagent level tributyl phosphate, technique is simple, and product purity is high, and operating condition is gentle, is adapted to The needs of scale industrial production.

Embodiment

Technical scheme of the present invention is further described with reference to specific embodiment.

Embodiment 1

A kind of purification process of SILVER REAGENT tributyl phosphate, specific preparation process are as follows：

(1) 3000ml tributyl phosphates are placed in beaker, add 1.2-1.5% nitric acid 300ml, stirring, liquid separation removes Nitric acid layer；

(2) 0.6-0.8% sodium hydroxide solution is used again, and continuous to wash 3 times, each 300ml, each sodium hydroxide is abandoned Go, then it is not aobvious alkaline with pure water to water layer PH；

(3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤- 0.08MPa, discards front-end volatiles 20-30ml, Produce, the positive cut of gained is detected according to GB/T15354-2011, up to 99.5%, content and impurity meet point its content Analyse pure standard.

The above-mentioned detailed description carried out with reference to embodiment to a kind of purification process of SILVER REAGENT tributyl phosphate, is explanation Property rather than it is limited, can include several embodiments according to limited scope, therefore of the invention overall not departing from Changing and modifications under design, should belong within protection scope of the present invention.

Claims (2)

1. A kind of 1. purification process of SILVER REAGENT tributyl phosphate, it is characterised in that：Specific preparation process is as follows：

   (1) 1.2-1.5% nitric acid is added into tributyl phosphate and is stirred, liquid separation removes nitric acid layer；

   (2) continuously being washed with 0.6-0.8% sodium hydroxide solution again, each sodium hydroxide discards, then with pure water extremely The not aobvious alkalescence of water layer PH；

   (3) and then oil reservoir is in distilling flask, is evaporated under reduced pressure under the conditions of≤- 0.08MPa, discards front-end volatiles, produce.
2. 2. the purification process of SILVER REAGENT tributyl phosphate according to claim 1, it is characterised in that：The tributyl phosphate Volume ratio with 1.2-1.5% nitric acid is 10:1.