CN108128802B - A kind of manufacture craft of pharmaceutical grade titanium dioxide - Google Patents
A kind of manufacture craft of pharmaceutical grade titanium dioxide Download PDFInfo
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- CN108128802B CN108128802B CN201810109784.XA CN201810109784A CN108128802B CN 108128802 B CN108128802 B CN 108128802B CN 201810109784 A CN201810109784 A CN 201810109784A CN 108128802 B CN108128802 B CN 108128802B
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- titanium
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- titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
- C01G23/0534—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts in the presence of seeds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to field of titanium more particularly to a kind of manufacture crafts of pharmaceutical grade titanium dioxide.The present invention uses high titanium slag titanium liquor manufacture method, solves Titanium in Ilmenite iron than technical problem low, more than impurity, has reached the technical effect that titanium liquid manufacturing cost is low, quality is high；Using alkaline process titanium white production technique, high titanium slag is reacted with sulfuric acid solution using NaOH dissolved salt, having reached can be by the technical effect of control sulfuric acid mass fraction and the titanium sulfate solution of the solid available difference F value of mass ratio of acid and mass concentration；Using the technical method by the way that aluminium alloy additive is added in hydrolytic process, the covering power for improving titanium dioxide, the technical effect of dispersibility and light resistance and the stability of the titanium dioxide increased are reached.
Description
Technical field
The present invention relates to field of titanium more particularly to a kind of manufacture crafts of pharmaceutical grade titanium dioxide.
Background technique
Medical grade titanium dioxide is the normal custom in food and medicine field compared with the anatase titanium dioxide of high score non-packet film process
Referred to as antholeucin is referred to as food-grade titanium dioxide or pharmaceutical grade titanium dioxide, eats titanium dioxide, also increases as food
White dose of use, nontoxic, tasteless, white powder sometimes disperse for convenience, are also made liquid, be widely used in pharmacy,
In foods and cosmetics industry.
And the titanium dioxide of high-purity is of wide application at present, in chemical reagent, medicine, food, cosmetics, electronics etc.
Aspect is all important industrial chemicals, these fields often require the content of titanium dioxide 98% or more.Because of the titanium dioxide of high-purity
Titanium have excellent pigment performance, the content of objectionable impurities is very low, thus can be used as medical product, be mainly used for various ointment,
Emulsifiable paste, creme, capsule, compressed powder ball, the sugar-coat of tablet and medical grade rubber, pharmaceutical plastic products, in medicinal ink；Because of its grain
Uniformly, good dispersion can be used as food titanium dioxide to degree, be mainly used for toothpaste, chocolate, food color, packaging for foodstuff material
Material and packing container etc..
Sulfuric acid method titanium pigment production is the technology that titanium dioxide manufacturer, China generally uses, and cardinal principle is to pass through titanium
Mine is mixed with sulfuric acid, is reacted, and titanium liquid is made, and then through processes such as sedimentation, heat filtering, crystallization, separation, refined filtration, concentrations, is improved black
The concentration and clarity of titanium liquid, remove ferrous iron therein, obtain the titanium liquid for meeting hydrolysis index.With the development of technology, external
Many titanium white production enterprises start the high titanium slag for using grade height, impurity few as the primary raw material of titanium white production.
It is existing medicine grade titanium dioxide there is no special preparation method, it be by industrial grade titanium dioxide into
Row detection, the product up to standard to some of ingredients are used as pharmaceutical grade.The medical titanium dioxide quality that this program obtains
Do not guarantee, and yield is not high, can be detected completely due to cannot be guaranteed all products, so hidden with certain safety
Suffer from.
Summary of the invention
The technical problems to be solved by the invention are to provide a kind of pharmaceutical grade titanium for above-mentioned technical deficiency
The manufacture craft of white powder is solved in ilmenite using high titanium slag titanium liquor manufacture method, and ferrotianium is asked than technology low, more than impurity
Topic, has reached the technical effect that titanium liquid manufacturing cost is low, quality is high；Using alkaline process titanium white production technique, NaOH dissolved salt is used
High titanium slag is reacted with sulfuric acid solution, having reached can be by control sulfuric acid mass fraction and the solid available difference F of mass ratio of acid
The technical effect of the titanium sulfate solution of value and mass concentration；Using the technology by the way that aluminium alloy additive is added in hydrolytic process
Method reaches the covering power for improving titanium dioxide, the technology of dispersibility and light resistance and the stability of the titanium dioxide increased
Effect；Simultaneously using alkaline process titanium dioxide manufacture craft and sulfuric acid method titanium pigment manufacture craft, reaches and improved this manufacture craft institute
Produce the technical effect of the quality of medical grade titanium dioxide.
In order to solve the above technical problems, the technical scheme adopted by the invention is that: include the following steps:
A, titanium ore is added in concentrated sulfuric acid A by sour mine ratio 1:1.5, is added and causes liquid, initiation reaction is heated by steam,
Concentrated sulfuric acid concentration is 92.5%-98%, and initiation temperature is 90 DEG C -120 DEG C, cures 3-5 hours after the reaction was completed, water logging is then added
It takes, obtains titanium liquid A；
1:6 reacts high titanium slag with NaOH fused salt in molar ratio, will obtain the washing of fused salt reaction product, and use sulfuric acid B
Dissolution washing product, obtains titanium liquid B；
B, titanium liquid A is mixed with titanium liquid B by 1:2 mass ratio, obtains mixed with titanium liquid C, titanium liquid C is concentrated, makes the total titanium of titanium liquid C
Concentration is 230g/L, and water bath with thermostatic control is preheated to 96 DEG C；
C, it removes ionized water, is added aluminium alloy additive and sodium sulphate, the molar ratio of aluminium alloy additive and sodium sulphate is
1:1 obtains solution D；
D, solution D is uniformly mixed than 1:4 by measure with titanium liquid C and is hydrolyzed, and stirred using blender, is heated to
Boiling stops heating when solution becomes steel grey, and stirring is slowed down, and keeps the temperature 30min, continues to be heated to boil again, hydrolyze
At obtaining metatitanic acid；
E, metatitanic acid progress pickling, bleaching, washing, salt treatment, calcining and pulverizer crush to obtain high-quality titanium dioxide.
The technical program is advanced optimized, the step A sulfuric acid B mass fraction is 43.4%, and the solid mass ratio of acid is 1:1.
The technical program is advanced optimized, sulfuric acid concentration after causing liquid is added in the step A and controls in 80%-90%,
For leaching temperature less than 80 DEG C, leaching time is five hours.
The technical program is advanced optimized, TiO in titanium ore in the step A2Content be greater than 50%, TiO in high titanium slag2
Content be greater than 75%.
The technical program is advanced optimized, aluminium alloy additive additive amount is contained in the step C with its metal oxide
Amount is standard, accounts for 0.3% of content of titanium dioxide in titanium liquid C.
The technical program is advanced optimized, deionized PH is preheated less than 2, and using constant temperature oil bath in the step C
To 96 DEG C.
The technical program is advanced optimized, the step D hydrolysis temperature is 110 DEG C, and the time is four hours.
Compared with prior art, the invention has the following advantages that the TiO2 grade of 1, titanium slag is high, impurity content significantly under
Drop, is conducive to the raising of titanium white powder yield；2, iron titanium ratio is low, and impurity content is few, and washing time and wastewater discharge also reduce；3,
The titanium dioxide optical catalyst for being added to aluminium alloy additive shows higher light absorpting ability than what is do not added；4, it adds
The product hydrolyzed after aluminium alloy additive afterwards, particle is more tiny, filtration time of the filtration time than conventional hydrolysis processes
It greatly increases；5, the content of the metal impurities such as iron, manganese, chromium, magnesium in titanium liquid is effectively reduced.
Detailed description of the invention
Fig. 1 is titanium liquid manufacturing process structure chart figure；
Fig. 2 is titanium hydrolysis process structure diagram；
Fig. 3 is that titanium dioxide generates subsequent flow；
Fig. 4 is the chemical equation figure in production process.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment and join
According to attached drawing, the present invention is described in more detail.It should be understood that these descriptions are merely illustrative, and it is not intended to limit this hair
Bright range.In addition, in the following description, descriptions of well-known structures and technologies are omitted, to avoid this is unnecessarily obscured
The concept of invention.
Specific embodiment 1: as shown in Figure 1-3, including the following steps:
A, titanium ore is added in concentrated sulfuric acid A by sour mine ratio 1:1.5, is added and causes liquid, initiation reaction is heated by steam,
Concentrated sulfuric acid concentration is 92.5%-98%, and initiation temperature is 90 DEG C -120 DEG C, cures 3-5 hours after the reaction was completed, water logging is then added
It takes, obtains titanium liquid A；
1:6 reacts high titanium slag with NaOH fused salt in molar ratio, and obtained fused salt reaction product is washed, and uses sulfuric acid
B dissolution washing product, obtains titanium liquid B；
B, titanium liquid A is mixed with titanium liquid B by 1:2 mass ratio, obtains mixed with titanium liquid C, titanium liquid C is concentrated, makes the total titanium of titanium liquid C
Concentration is 230g/L, and water bath with thermostatic control is preheated to 96 DEG C；
C, it removes ionized water, is added aluminium alloy additive and sodium sulphate, the molar ratio of aluminium alloy additive and sodium sulphate is
1:1 obtains solution D；
D, solution D is uniformly mixed than 1:4 by measure with titanium liquid C and is hydrolyzed, and stirred using blender, is heated to
Boiling stops heating when solution becomes steel grey, and stirring is slowed down, and keeps the temperature 30min, continues to be heated to boil again, hydrolyze
At obtaining metatitanic acid；
E, metatitanic acid progress pickling, bleaching, washing, salt treatment, calcining and pulverizer crush to obtain high-quality titanium dioxide；
The step A sulfuric acid B mass fraction is 43.4%, and the solid mass ratio of acid is 1:1；Sulfuric acid after causing liquid is added in the step A
Concentration is controlled in 80%-90%, and for leaching temperature less than 80 DEG C, the recovery time is five hours；TiO in titanium ore in the step A2's
Content is greater than 50%, TiO in high titanium slag2Content be greater than 75%；Aluminium alloy additive additive amount is in the step C with its metal
Oxide content is standard, accounts for 0.3% of content of titanium dioxide in titanium liquid C；Deionized PH is less than 2 in the step C, and
96 DEG C are preheated to using constant temperature oil bath；The step D hydrolysis temperature is 110 DEG C, and the time is four hours.
In Fig. 1, titanium liquid necessary to production titanium dioxide is made by two ways, first way is the same as traditional sulfuric acid process
It is identical to make titanium liquid mode, generates titanium liquid using titanium ore and strong sulfuric acid response；And the second way is high using grade, impurity is few
Primary raw material of the high titanium slag as titanium dioxide production, the main component of high titanium slag are Ti3O5, Ti3O5In NaOH fused salt
The reaction such as Fig. 4 Chinese style 1-2 occurs, and after washing solid phase (xNa2O·TiO2·yH2O) titanium sulfate is formed with sulfuric acid reaction
Solution, reaction equation such as formula 1-3 can pass through control sulfuric acid mass fraction and the solid available difference F value of mass ratio of acid and matter
The titanium sulfate solution for measuring concentration, titanium liquid required for must wanting；And titanium liquid is prepared by titanium ore simultaneously, the formula 1-1 in principle such as Fig. 4,
Two kinds of titanium liquid are mixed, impurity content can be reduced by high titanium slag titanium liquid and yield is improved by titanium ore titanium liquid, in conjunction with
The two advantage provides condition to obtain the titanium dioxide of high-quality, and production cost is all lower than titanium ore and high titanium slag is used alone；Together
When combine alkaline process titanium dioxide manufacture craft and sulfuric acid method titanium pigment manufacture craft, improve the produced pharmaceutical grade two of this manufacture craft
The quality of titanium oxide.
Fig. 2 be titanium dioxide generate in most important hydrolytic process, hydrolyze equation such as Fig. 4 Chinese style 1-4, the present invention by
Additive is added in hydrolytic process to improve the pigment performance of titanium dioxide, and this step is combined with hydrolysis process,
Exactly introduce aluminium alloy additive in titanium hydrolysis, on the basis of existing hydrolysis process be made titanium dioxide, the purpose is to
Aluminium alloy additive all replaces automatic growing crystal species or initiation and regulator as automatic growing crystal species to add to inducing action has been hydrolyzed
A small amount of additive can improve the covering power of titanium dioxide, dispersibility and light resistance.In addition, the titanium dioxide being added to it is steady
It is qualitative higher than what is do not added, a certain amount of aluminium alloy additive is added in deionized water first, aluminium alloy additive
Additive amount is to account for 3% or so of content of titanium dioxide in titanium liquid using its metal oxide as standard, and add in deionized water
The effect for entering sodium sulphate and resisting with this other ions achievees the purpose that eliminate other impurities.
Then the titanium liquid after preheating is added in two steps in the deionized water containing aluminium alloy additive and vulcanized sodium: first
The 10% of titanium liquid measure is added in step, keeps the temperature 5-10min;Second step rapidly joins residual titanium liquid, and heating rate is fast, is heated to boiling
It rises, when solution colour becomes steel grey, stops heating, stirring slows down, and keeps the temperature 20-30min, continues to be heated to boil again.
When closing to an end wait react, it is slowly added to boiling water so that reaction is more complete.The entire reaction time is 4 hours.It obtains herein miscellaneous
Matter is few, the higher metatitanic acid hydrolysate of purity；
Such as Fig. 3, after obtaining metatitanic acid product, subsequent step is identical as traditional silicon dioxide manufacture craft, i.e., pickling,
Bleaching, washing, salt treatment, calcining and pulverizer crush these steps, finally obtain pharmaceutical grade anatase titanium dioxide, and make
Content of titanium dioxide reaches medical standard；Fig. 4 Chinese style 1-5 is that calcinated titanium dioxide generates reaction equation.
And salt used in salt treatment process is sylvite potassium carbonate, potassium sulfate and potassium acid sulfate, sylvite is to this production of improvement
The pigment performance of technique has very big benefit, and particle can be made loose, improves whiteness and reducing power, can make titanium dioxide compared with
Calcining is without losing excellent pigment performance under high-temperature, because titanium dioxide granule compares cause when calcining at relatively high temperatures
It is close, be conducive to improve weatherability and reduce oil absorption.The additive amount of sylvite is generally TiO20.25% ~ 0.70% (with K2O meter).
Phosphoric acid can improve product whiteness and weatherability, and particle is softer, be easy to crush.(in terms of) that additive amount is generally；In addition, phosphorus
Acid can also eliminate the influence of iron tramp, soluble titanium and heavy metal element.Zinc chloride adds in this manufacture craft salt treatment
0.15%, potassium carbonate addition 0.25%, phosphoric acid,diluted addition 0.15%.
And last process, Calcine Strength manufacture result is influenced it is maximum, when higher calcination temperature and longer heat preservation
Between can obtain higher whiteness, pH value.This manufacture craft determines that optimum calcinating temperature is 870 DEG C, and best soaking time is two
Hour.
It should be understood that above-mentioned specific embodiment of the invention is used only for exemplary illustration or explains of the invention
Principle, but not to limit the present invention.Therefore, that is done without departing from the spirit and scope of the present invention is any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.In addition, appended claims purport of the present invention
Covering the whole variations fallen into attached claim scope and boundary or this range and the equivalent form on boundary and is repairing
Change example.
Claims (2)
1. a kind of manufacture craft of pharmaceutical grade titanium dioxide, characterized by the following steps:
A, titanium ore is added in concentrated sulfuric acid A by sour mine ratio 1:1.5, is added and causes liquid, initiation reaction, dense sulphur are heated by steam
Acid concentration is 92.5%-98%, and initiation temperature is 90 DEG C -120 DEG C, cures 3-5 hours after the reaction was completed, water extraction is then added,
Obtain titanium liquid A；
1:6 reacts high titanium slag with NaOH fused salt in molar ratio, and gained fused salt reaction product is washed, and is dissolved using sulfuric acid B
Product is washed, titanium liquid B is obtained；
B, titanium liquid A is mixed with titanium liquid B by 1:2 mass ratio, obtains mixed with titanium liquid C, titanium liquid C is concentrated, makes the total titanium concentration of titanium liquid C
230g/L, and water bath with thermostatic control is preheated to 96 DEG C；
C, it removes ionized water, is added aluminium alloy additive and sodium sulphate, the molar ratio of aluminium alloy additive and sodium sulphate is 1:1,
Obtain solution D；
D, solution D is uniformly mixed than 1:4 by measure with titanium liquid C and is hydrolyzed, and stirred using blender, be heated to boiling,
When solution becomes steel grey, stop heating, stirring is slowed down, and is kept the temperature 30min, is continued to be heated to boil again, and hydrolysis is completed
To metatitanic acid；
E, metatitanic acid progress pickling, bleaching, washing, salt treatment, calcining and pulverizer crush to obtain high-quality titanium dioxide；
Step A sulfuric acid B mass fraction is 43.4%, and the solid mass ratio of acid is 1:1；
Sulfuric acid concentration after causing liquid is added in step A to control in 80%-90%, for leaching temperature less than 80 DEG C, leaching time is five small
When;
TiO in titanium ore in step A2Content be greater than 50%, TiO in high titanium slag2Content be greater than 75%;
Aluminium alloy additive additive amount accounts for content of titanium dioxide in titanium liquid C using its metal oxide content as standard in step C
0.3%。
2. a kind of manufacture craft of pharmaceutical grade titanium dioxide according to claim 1, it is characterised in that: step D hydrolysis temperature
It is 110 DEG C, the time is four hours.
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| CN201810109784.XA CN108128802B (en) | 2017-02-02 | 2017-02-02 | A kind of manufacture craft of pharmaceutical grade titanium dioxide |
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| CN201710062306.3A CN106745229B (en) | 2017-02-02 | 2017-02-02 | A kind of manufacture craft of pharmaceutical grade titanium dioxide |
| CN201810109784.XA CN108128802B (en) | 2017-02-02 | 2017-02-02 | A kind of manufacture craft of pharmaceutical grade titanium dioxide |
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| CN108128802B true CN108128802B (en) | 2019-11-29 |
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| CN201710062306.3A Active CN106745229B (en) | 2017-02-02 | 2017-02-02 | A kind of manufacture craft of pharmaceutical grade titanium dioxide |
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| CN107500346B (en) * | 2017-09-01 | 2019-06-07 | 河北麦森钛白粉有限公司 | A kind of method for preparing raw material for decorating base paper titanium white production |
| CN114162853A (en) * | 2021-12-10 | 2022-03-11 | 长沙华希新材料有限公司 | Hydrolysis process for preparing metallurgical titanium dioxide for hard alloy |
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| CN101172648A (en) * | 2006-10-30 | 2008-05-07 | 中国科学院过程工程研究所 | Method for clean production of titanium dioxide by using sodium hydroxide |
| CN101514031A (en) * | 2008-02-18 | 2009-08-26 | 四川龙蟒钛业股份有限公司 | Titanium ore acidolysis method through sulfuric acid process |
| CN103194603A (en) * | 2013-04-01 | 2013-07-10 | 攀枝花学院 | Preparation method of high-purity vanadium pentoxide |
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| AUPR820301A0 (en) * | 2001-10-12 | 2001-11-01 | Rmg Services Pty. Ltd. | Treatment of a wide range of titanium oxide compounds |
| US7008602B2 (en) * | 2002-04-19 | 2006-03-07 | Millennium Inorganic Chemicals, Inc. | Beneficiation of titaniferous ore with sulfuric acid |
| CN101994012B (en) * | 2010-12-07 | 2012-08-29 | 东北大学 | Method for producing titanium dioxide by using titanium-containing blast furnace slag |
| CN103723765B (en) * | 2014-01-20 | 2015-04-22 | 韶关学院 | Method for preparing titanium dioxide through sulfuric acid method |
| CN103922396B (en) * | 2014-04-02 | 2015-08-19 | 济南裕兴化工有限责任公司 | The technique of rutile titanium white powder produced by a kind of low-grade titanium ore |
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| CN101172648A (en) * | 2006-10-30 | 2008-05-07 | 中国科学院过程工程研究所 | Method for clean production of titanium dioxide by using sodium hydroxide |
| CN101514031A (en) * | 2008-02-18 | 2009-08-26 | 四川龙蟒钛业股份有限公司 | Titanium ore acidolysis method through sulfuric acid process |
| CN103194603A (en) * | 2013-04-01 | 2013-07-10 | 攀枝花学院 | Preparation method of high-purity vanadium pentoxide |
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| CN108128802A (en) | 2018-06-08 |
| CN106745229A (en) | 2017-05-31 |
| CN106745229B (en) | 2018-07-31 |
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