WO2018039847A1

WO2018039847A1 - Method for preparing titanyl sulfate

Info

Publication number: WO2018039847A1
Application number: PCT/CN2016/097111
Authority: WO
Inventors: 沈建美
Original assignee: 沈建美
Priority date: 2016-08-29
Filing date: 2016-08-29
Publication date: 2018-03-08

Abstract

Provided is a method for preparing titanyl sulfate. The method comprises the following steps: sequentially adding a metatitanic acid solid and sulfuric acid to a reaction kettle, stirring into a slurry without obvious hard lumps, then adding titanyl sulfate crystal seeds, and maintaining the temperature to precipitate crystals; the addition amount of crystal seeds is 0.23 percent of the mass of the metatitanic acid, the crystal seeds are pure titanyl sulfate crystals with a uniform texture and with a crystal size not exceeding 0.1 mm; and cooling the crystallization solution to room temperature, carrying out vacuum suction filtration or centrifuge filtration, and separating out a mother liquor to obtain titanyl sulfate crystals. The advantages thereof lie in that the method using a rational adjusting technology realizes the preparation of titanyl sulfate under conditions of a low temperature and a low concentration, and the prepared titanyl sulfate has greatly improved water solubility, and facilitates the preparation of titanyl sulfate downstream products.

Description

[Invention name established by ISA according to Rule 37.2] Method for preparing titanium oxysulfate

Method for detecting moisture content of crude oil

Technical field

The invention belongs to the field of chemical processes, and in particular relates to a method for detecting the moisture content of crude oil.

Background technique

The sulfates of titanium are titanium sulfate and titanium oxysulfate, namely Ti(SO4)2 and TiOSO2. According to the formula, the titanium content of titanium sulfate is only 20%, and the titanium content of titanium oxysulfate is as high as 30%. Then for titanium aqueous solutions, titanium oxysulfate can provide a more sufficient amount of titanium source, which provides great convenience for downstream products and saves the cost of removing a large amount of sulfate in the solution. The preparation of nano-sized titanium dioxide by using titanium oxysulfate can effectively reduce the agglomeration of nano-sized titanium dioxide particles, improve the dispersibility and improve the catalytic effect.

Summary of the invention

The object of the present invention is to provide a method for detecting the moisture content of crude oil in view of the deficiencies of the prior art.

In order to achieve the above object, the technical solution of the present invention is: a method for detecting the moisture content of crude oil, which is innovative in that it comprises the following preparation steps:

(1) The titanic acid solid and the sulfuric acid having a concentration of 40% are sequentially put into the reaction vessel, and stirred until there is no obvious hard block, which is a uniform slurry, wherein the mass ratio of the metatitanic acid to the sulfuric acid after dehydration is 1 :5;

(2) adding an acidification aid of 6% by weight of metatitanic acid to the slurry of the upper step; the acidification aid is a mixture of sulfuric acid, an oxidant and water, wherein the oxidant is at a concentration of 45% Aqueous hydrogen peroxide solution;

(3) The temperature of the solution is lowered to 50 ° C, and then the seed crystal of titanyl sulfate is added to precipitate crystals; the seed crystal is added in an amount of 0.25% by mass of the metatitanic acid, and the seed crystal is uniform and pure in texture. a titanyl sulfate crystal having a crystal grain size of not more than 0.1 mm;

(4) After the crystallizing liquid is cooled to room temperature, vacuum filtration or centrifugal filtration, and the mother liquid is separated to obtain a titanyl sulfate crystal.

The beneficial effects of the invention are as follows: the invention realizes the preparation of titanyl sulfate under the conditions of low temperature and low concentration by rationally adjusting the process, and the prepared water-soluble titanium oxysulfate is greatly improved in water solubility, and is favorable for the preparation of the product of the titanium oxysulfate downstream.

detailed description

The embodiments of the present invention are described below by way of specific embodiments, and those skilled in the art can readily understand other advantages and functions of the present invention from the disclosure.

Example 1

A method for preparing titanyl sulfate comprises the following preparation steps:

(1) The titanic acid solid and the sulfuric acid having a concentration of 40% are sequentially put into the reaction vessel, and stirred until there is no obvious hard block, which is a uniform slurry, wherein the mass ratio of metatitanic acid to sulfuric acid after deionization is 1:5. ;

(2) adding an acidification aid of 6% by weight of metatitanic acid to the slurry of the previous step; the acidification aid is a mixture of sulfuric acid, an oxidant and water, wherein the oxidant is a 45% aqueous solution of hydrogen peroxide, and the water is deionized. Water, sulfuric acid, oxidant and water are mixed in a mass ratio of 5:1:15;

(3) The temperature of the solution is lowered to 50 ° C, and then the seed crystal of titanyl sulfate is added to precipitate crystals; the seed crystal is added in an amount of 0.2% by mass of metatitanic acid, and the seed crystal is a uniform and pure titanium oxide sulfate. Crystal, the crystal grain size of which does not exceed 0.1 mm;

Claims

A method for detecting the moisture content of crude oil, comprising the following steps of preparing:

(1) The titanic acid solid and the sulfuric acid having a concentration of 40% are sequentially put into the reaction vessel, and stirred until there is no obvious hard block, which is a uniform slurry, wherein the mass ratio of the metatitanic acid to the sulfuric acid after dehydration is 1 :5;

(2) adding an acidification aid of 6% by weight of metatitanic acid to the slurry of the upper step; the acidification aid is a mixture of sulfuric acid, an oxidant and water, wherein the oxidant is at a concentration of 45% Aqueous hydrogen peroxide solution;

(3) The temperature of the solution is lowered to 50 ° C, and then the seed crystal of titanyl sulfate is added to precipitate crystals; the seed crystal is added in an amount of 0.25% by mass of the metatitanic acid, and the seed crystal is uniform and pure in texture. a titanyl sulfate crystal having a crystal grain size of not more than 0.1 mm;

(4) After the crystallizing liquid is cooled to room temperature, vacuum filtration or centrifugal filtration, and the mother liquid is separated to obtain a titanyl sulfate crystal.