CN109943103A - The preparation method and applications of rutile type titanium white - Google Patents
The preparation method and applications of rutile type titanium white Download PDFInfo
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- CN109943103A CN109943103A CN201910306117.5A CN201910306117A CN109943103A CN 109943103 A CN109943103 A CN 109943103A CN 201910306117 A CN201910306117 A CN 201910306117A CN 109943103 A CN109943103 A CN 109943103A
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Abstract
This application involves a kind of preparation method and applications of rutile type titanium white, belong to titanium dioxide preparation technical field.A kind of preparation method of rutile type titanium white, including dichloro oxygen titanium is hydrolyzed with mixing bottom liquid and mix under preset temperature, hydrolysate is separated into obtain rutile-type hydrated titanium dioxide, then calcined.Mixing bottom liquid includes hydrochloric acid, surfactant and water.The application uses dichloro oxygen titanium self-seed pressure hydrolysis, by the hydrogen ion concentration in control mixing bottom liquid, the hydrated titanium dioxide of Rutile Type is directly generated, pure rutile type titanium dioxide can be obtained by low temperature calcination dehydration, process flow is simple, and the reaction time is short.
Description
Technical field
This application involves titanium dioxide preparation technical fields, and the preparation method of in particular to a kind of rutile type titanium white and
It is applied.
Background technique
Titanium dioxide (TiO2) be a kind of important inorganic chemical product, coating, ink, papermaking, plastic, rubber, chemical fibre,
There is important use in the industry such as ceramics.The industrialized preparing process of titanium dioxide common are sulfuric acid process and chloridising.Chloridising pair
Raw material require height, and also high to equipment corrosion resistance, technical difficulty is big.The preparation of sulfuric acid process crystal seed is complicated, and energy consumption is high.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the embodiment of the present application includes providing a kind of preparation of rutile type titanium white
Method and its application, process flow are simple.
In a first aspect, the embodiment of the present application proposes a kind of preparation method of rutile type titanium white, comprising: by dichloro oxygen
Titanium is hydrolyzed with mixing bottom liquid and mix under preset temperature, and hydrolysate is separated to obtain rutile-type hydrated titanium dioxide, then
It is calcined.Mixing bottom liquid includes hydrochloric acid, surfactant and water.
The application uses dichloro oxygen titanium self-seed pressure hydrolysis, by the hydrogen ion concentration in control mixing bottom liquid, directly
The hydrated titanium dioxide for delivering a child into Rutile Type can be obtained pure rutile type titanium dioxide, technique stream by low temperature calcination dehydration
Journey is simple, and the reaction time is short.Crystal seed is prepared it is not necessary that lye is added in this method production process, moreover it is possible to be recycled a large amount of hydrochloric acid, be realized
The comprehensive utilization of resource, reduces the pollution to environment.
In the section Example of the application, dichloro oxygen titanium is 3-5:1 with the volume ratio for mixing bottom liquid.
The proportion so that dichloro oxygen titanium mixing bottom liquid in can be fully hydrolyzed generation crystal seed, avoid the improper shadow of reaction ratio
Ring the generation quality of crystal seed.
In the section Example of the application, dichloro oxygen titanium with mix bottom liquid under conditions of 80-110 DEG C and hydrolyze 2-3 it is small
When.
Pass through H in control mixing bottom liquid+Concentration, dichloro oxygen titanium hydrolytic process is relatively slow, hydrolyzes the complex ion of generation
Crystallization occurs in polycondensation process for unit, and forms multidimensional hydroxyl bridge, directly generates the hydrated titanium dioxide of Rutile Type.In water
During solution, because of not containing sulfate radicals in system, anion coordination-polyhedron not will form, to inhibit anatase titanium dioxide TiO2's
Oxolation is formed.
In the section Example of the application, dichloro oxygen titanium is preheated to 80-98 DEG C with bottom liquid is mixed respectively before mixing.
By dichloro oxygen titanium with to mix bottom liquid to be preheated to 80-98 DEG C respectively be to mix dichloro oxygen titanium with bottom liquid is mixed
Moment hydrolysis generates crystal seed, so that dichloro oxygen titanium be avoided, from the irregular crystal seed of hydrolysis, to influence product matter under the conditions of no crystal seed
Amount.
In the section Example of the application, the dichloro oxygen titanium of preheating is 15-20min with the incorporation time for mixing bottom liquid.
Dichloro oxygen titanium can be made sufficiently to react with bottom liquid is mixed with speed mixing, crystal seed in guarantee hydrolytic process
It generates, addition speed is excessively slow, and the crystal seed of generation is few, and partial size is big；Then there may be irregular crystal seeds for excessive velocities.
In the section Example of the application, for dichloro oxygen titanium concentration in terms of titanium dioxide, the concentration of titanium dioxide is 200-
300g/L。
The dichloro oxygen titanium of the concentration with it is above-mentioned mix bottom liquid mixing after, generation crystallization can be fully hydrolyzed.
In the section Example of the application, rutile-type hydrated titanium dioxide calcines 20- under conditions of 400-600 DEG C
40min。
Calcining is and then to obtain pure rutile titanium dioxide to remove the moisture in the hydrated titanium dioxide of Rutile Type
Powder.
In the section Example of the application, the concentration for mixing the hydrochloric acid in the liquid of bottom is 0.1-1mol/L.
Hydrochloric acid is used to adjust the pH value of mixing bottom liquid, H in control mixing bottom liquid+Concentration, and then control Rutile Type
The formation of hydrated titanium dioxide.
In the section Example of the application, the mass percentage of surfactant is 0.1-2%.Optionally, surface
Activating agent includes in cetyltrimethylammonium bromide, neopelex, dodecyl sodium sulfate and polyethylene glycol
At least one.
Surfactant is used to control the mixing dispersing uniformity of mixing bottom liquid and dichloro oxygen titanium, avoids in mixed process
Reunite, the reunion situation in notice control crystal seed forming process.
Second aspect, the embodiment of the present application propose the rutile as made from the preparation method of above-mentioned rutile type titanium white
Application of the type titanium dioxide in coating, ink, papermaking, plastic, rubber, chemical fibre and ceramic field.
Detailed description of the invention
Technical solution in ord to more clearly illustrate embodiments of the present application, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only some embodiments of the application, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the XRD diagram for the rutile type titanium white that the embodiment of the present application 1 provides；
Fig. 2 is the XRD diagram for the rutile type titanium white that the application comparative example provides.
Specific embodiment
It, below will be in the embodiment of the present application to keep the purposes, technical schemes and advantages of the embodiment of the present application clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
The industrialized preparing process of titanium dioxide common are sulfuric acid process and chloridising.Sulfuric acid process is with sulfuric acid solution containing titanium ore
Object obtains titanyl sulfate solution, and purified and hydrolysis obtains metatitanic acid precipitating, enters back into brickkiln roasting output titanium dioxide pigment
The step of product is non-continuous production processes, and process flow is complicated, needs 20 or so, discharge waste is more, crystal transfer
Multioperation step is needed, the burning process of use needs to consume mass energy.
In method for producing gtitanium dioxide with sulphuric acid, rutile type titanium generally is prepared by two methods of automatic growing crystal species and plus seed
White powder.When plus seed, domestic and international many enterprises are used in TiCl4It is added in alkali (sodium hydroxide, ammonium hydroxide, urea etc.) in solution
With, rutile-type hydrolysis crystal seed is generated, but because of the influence of factors, the rutile type titanium white quality fluctuation of preparation is larger,
It is less reproducible；And automatic growing crystal species are usually to generally require outside in salt treatment plus calcine rutilization nuclei, in higher temperature
The lower calcining of degree can just obtain rutile type titanium white, and crystal seed preparation is complicated, and energy consumption is high, at high cost.
Chloridising is to generate four chlorinations with ilmenite, high titanium slag, synthetic rutile or natural rutile etc. and chlorine reaction
Titanium through rectification and purification, then carries out gaseous oxidation, after quickly cooling, obtains titanium dioxide by gas solid separation, requires height to raw material,
Also high to equipment corrosion resistance, technical difficulty is big.
A kind of preparation method and applications of rutile type titanium white of the embodiment of the present application are specifically described below.
The embodiment of the present application proposes a kind of preparation method of rutile type titanium white, comprising: by dichloro oxygen titanium with mix
Bottom liquid is mixed under preset temperature and is hydrolyzed, and hydrolysate is separated to obtain rutile-type hydrated titanium dioxide, then calcined.
In the section Example of the application, hydrochloric acid, surfactant and water are mixed in a certain ratio to obtain mixing bottom
Liquid, by the mixing bottom, liquid is put into reaction kettle, is opened stirring, is heated to 80-98 DEG C.
In the embodiment of the present application, hydrochloric acid is used to adjust the pH value of mixing bottom liquid, H in control mixing bottom liquid+Concentration, dichloro
Oxygen titanium hydrolytic process is relatively slow, and then controls the formation of the hydrated titanium dioxide of Rutile Type.In embodiment in the cards
In, the concentration for mixing the hydrochloric acid in the liquid of bottom is 0.1-1mol/L.Optionally, the concentration of hydrochloric acid can be 0.2mol/L, 0.3mol/
L,0.5mol/L,0.8mol/L.It should be noted that the dichloro oxygen titanium in the application is outsourcing, had by Fujian richness bodyguard new material
It limit responsible company to provide, be extracted by ilmenite.In actual application, dichloro oxygen titanium, the application couple can also be made by oneself
It is without limitation.
In the embodiment of the present application, surfactant is uniformly dispersed for controlling mixing bottom liquid and the mixing of dichloro oxygen titanium
Property, it avoids reuniting in mixed process, while also controlling the reunion situation in crystal seed forming process.Implement the application part
In example, the mass percentage of surfactant is 0.1-2%.Optionally, mass percentage 0.5%, 1%, 1.5%.
In the application section Example, surfactant includes cetyltrimethylammonium bromide, neopelex, dodecane
At least one of base sodium sulfonate and polyethylene glycol.
By dichloro oxygen titanium with to mix bottom liquid to be preheated to 80-98 DEG C respectively be to mix dichloro oxygen titanium with bottom liquid is mixed
Moment hydrolysis generates crystal seed, so that dichloro oxygen titanium be avoided, from the irregular crystal seed of hydrolysis, to influence product matter under the conditions of no crystal seed
Amount.
In embodiments herein, for dichloro oxygen titanium concentration in terms of titanium dioxide, the concentration of titanium dioxide is 200-300g/
L.The dichloro oxygen titanium of the concentration with it is above-mentioned mix bottom liquid mixing after, generation crystallization can be fully hydrolyzed, obtain the golden red of high quality
The hydrated titanium dioxide of stone phase.Optionally, the concentration of titanium dioxide can be 220g/L, 250g/L, 280g/L.
Mixing bottom liquid by the dichloro oxygen titanium by preheating with certain speed and by preheating mixes, in 80-110 DEG C of item
It is hydrolyzed 2-3 hours under part.Pass through H in control mixing bottom liquid+Concentration, dichloro oxygen titanium hydrolytic process is relatively slow, hydrolysis generate
Complex ion unit crystallization occurs in polycondensation process, and form multidimensional hydroxyl bridge, directly generate the hydration dioxy of Rutile Type
Change titanium.During hydrolysis, because of not containing sulfate radicals in system, anion coordination-polyhedron not will form, to inhibit sharp
Titanium-type TiO2Oxolation formed.The reaction of hydrolysis are as follows:
TiOCl2+2H2O=TiO (OH)2+2HCl
In the section Example of the application, dichloro oxygen titanium is 3-5:1 with the volume ratio for mixing bottom liquid.The proportion is so that two
Chlorine oxygen titanium can be fully hydrolyzed generation crystal seed in mixing bottom liquid, avoid the generation quality of reaction ratio undue influence crystal seed.It can
Choosing, dichloro oxygen titanium is 4:1 with the volume ratio for mixing bottom liquid.
In the section Example of the application, hydrolyzed to guarantee dichloro oxygen titanium with sufficiently reacting for bottom liquid, guarantee is mixed
The generation quality of crystal seed in the process, the dichloro oxygen titanium aqueous solution after preheating are added in the bottom liquid after preheating, the time being added
It needs to control in 15-20min.
Hydrolysate is filtered by vacuum, separation hydrochloric acid obtains rutile-type hydrated titanium dioxide.Vacuum filtration can also
Using other methods such as centrifugations.
Rutile-type hydrated titanium dioxide is passed through salt treatment, is put by the high rutile type titanium white of quality in order to obtain
Calcined dehydration 20-40min is carried out in 400-600 DEG C of Muffle furnace, obtains pure rutile type titanium dioxide.Calcination reaction are as follows:
TiO(OH)2=TiO2+H2O
Wherein, calcination temperature can be 450 DEG C, 500 DEG C, 550 DEG C, and calcination time can be 25min, 30min, 35min.
In the section Example of the application, salt treatment are as follows: hydrated titanium dioxide is beaten, be added potassium sulfate, aluminum sulfate and
Phosphoric acid etc. is mixed 30 minutes.Wherein, the additional amount of potassium sulfate, aluminum sulfate and phosphoric acid need to be controlled, and avoid influencing titanium white
The performance of powder.
The addition of potassium sulfate can reduce calcination temperature, avoid product metachromatism caused by high temperature sintering.Phosphoric acid can be with
Improve the whiteness and weatherability of titanium dioxide.
The preparation method of rutile type titanium white provided by the present application uses dichloro oxygen titanium self-seed pressure hydrolysis, passes through
The hydrogen ion concentration of control mixing bottom liquid, directly generates the hydrated titanium dioxide of Rutile Type, is dehydrated by low temperature calcination
Pure rutile type titanium dioxide is obtained, process flow is simple, and the reaction time is short.It is not necessary that lye preparation is added in this method production process
Crystal seed, moreover it is possible to recycle a large amount of hydrochloric acid, realize the comprehensive utilization of resource, reduce the pollution to environment.
Second aspect, the purity is high of the rutile type titanium white as made from the preparation method of above-mentioned rutile type titanium white, can
To be applied to coating, ink, papermaking, plastic, rubber, chemical fibre and ceramic field.
The feature of the application and performance are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of preparation methods of rutile type titanium white, comprising:
The hydrochloric acid of 0.5mol/L and 1% neopelex are added in 100ml deionized water, in stirring condition
Under be heated to 94 DEG C.
The dichloro oxygen titanium of 400ml 250g/L containing titanium dioxide is preheated to 94 DEG C, and is added to preheating in 17 minutes
It mixes in the liquid of bottom.Continue after being warming up to 105 DEG C, heat preservation 2.5 hours, refrigerated separation obtains rutile-type hydrated titanium dioxide and salt
Acid.
It will be sent into 500 DEG C of Muffle furnace after hydrolysate progress salt treatment after calcining 30min and obtain rutile titanium dioxide
Powder.
Embodiment 2
The present embodiment provides a kind of preparation methods of rutile type titanium white, comprising:
The hydrochloric acid of 0.1mol/L and 2% cetyltrimethylammonium bromide are added in 100ml deionized water, is stirring
Under the conditions of be heated to 80 DEG C.
The dichloro oxygen titanium of 300ml 250g/L containing titanium dioxide is preheated to 90 DEG C, and is added to preheating in 15 minutes
It mixes in the liquid of bottom.Continue after being warming up to 90 DEG C, heat preservation 2 hours, refrigerated separation obtains rutile-type hydrated titanium dioxide and hydrochloric acid.
It will be sent into 400 DEG C of Muffle furnace after hydrolysate progress salt treatment after calcining 30min and obtain rutile titanium dioxide
Powder.
Embodiment 3
The present embodiment provides a kind of preparation methods of rutile type titanium white, comprising:
The hydrochloric acid of 1mol/L and 0.5% polyethylene glycol are added in 100ml deionized water, is added under agitation
Heat is to 98 DEG C.
The dichloro oxygen titanium of 500ml 250g/L containing titanium dioxide is preheated to 80 DEG C, and is added to preheating in 20 minutes
It mixes in the liquid of bottom；Continue after being warming up to 100 DEG C, heat preservation 3 hours, refrigerated separation obtains rutile-type hydrated titanium dioxide and salt
Acid.
Be sent into after salt treatment calcine 30min in 600 DEG C of Muffle furnace after obtain rutile type titanium white.
Embodiment 4
The present embodiment provides a kind of preparation methods of rutile type titanium white, comprising:
The hydrochloric acid of 1mol/L and 0.5% polyethylene glycol are added in 100ml deionized water, is added under agitation
Heat is to 98 DEG C.
The dichloro oxygen titanium of 500ml 250g/L containing titanium dioxide is preheated to 98 DEG C, and is added to preheating in 20 minutes
It mixes in the liquid of bottom；Continue after being warming up to 110 DEG C, heat preservation 3 hours, refrigerated separation obtains rutile-type hydrated titanium dioxide and salt
Acid.
Be sent into after salt treatment calcine 30min in 600 DEG C of Muffle furnace after obtain rutile type titanium white.
Comparative example
This comparative example provides a kind of preparation method of rutile type titanium white, difference from example 1 is that,
Hydrochloric acid and neopelex are not added in 100ml deionized water.
Test example
X-ray diffraction detection is carried out to the rutile type titanium white of Examples 1 to 4, comparative example preparation.Embodiment 1 provides
Rutile type titanium white result as shown in Figure 1, from XRD diagram as can be seen that its rutile type titanium white content be
100%.The XRD diagram for the rutile type titanium white that embodiment 2~4 provides is same as Example 1, illustrates its rutile-type obtained
Titanium white powder content is 100%.
The difference of the testing result of the rutile type titanium white of comparative example and embodiment 1 has impurity in the XRD diagram measured
Peak, as a result as shown in Fig. 2, illustrating that its product obtained is not pure products.
Embodiments described above is some embodiments of the present application, instead of all the embodiments.The reality of the application
The detailed description for applying example is not intended to limit claimed scope of the present application, but is merely representative of the selected implementation of the application
Example.Based on the embodiment in the application, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall in the protection scope of this application.
Claims (10)
1. a kind of preparation method of rutile type titanium white characterized by comprising
Dichloro oxygen titanium is hydrolyzed with mixing bottom liquid and mix under preset temperature, hydrolysate is separated to obtain rutile-type and be hydrated
Titanium dioxide, then calcined；
Mixing bottom liquid includes hydrochloric acid, surfactant and water.
2. the preparation method of rutile type titanium white according to claim 1, which is characterized in that the dichloro oxygen titanium and institute
The volume ratio for stating mixing bottom liquid is 3-5:1.
3. the preparation method of rutile type titanium white according to claim 1, which is characterized in that the dichloro oxygen titanium and institute
Mixing bottom liquid is stated to hydrolyze 2-3 hours under conditions of 80-110 DEG C.
4. the preparation method of rutile type titanium white according to claim 3, which is characterized in that the dichloro oxygen titanium and institute
It states mixing bottom liquid and is preheated to 80-98 DEG C respectively before mixing.
5. the preparation method of rutile type titanium white according to claim 4, which is characterized in that the dichloro oxygen of preheating
Titanium is 15-20min with the incorporation time for mixing bottom liquid.
6. the preparation method of rutile type titanium white according to claim 1, which is characterized in that the dichloro oxygen titanium concentration
In terms of titanium dioxide, the concentration of the titanium dioxide is 200-300g/L.
7. the preparation method of rutile type titanium white according to claim 1, which is characterized in that the rutile-type hydration
Titanium dioxide calcines 20-40min under conditions of 400-600 DEG C.
8. the preparation method of rutile type titanium white according to claim 1, which is characterized in that in the liquid of the mixing bottom
The concentration of the hydrochloric acid is 0.1-1mol/L.
9. the preparation method of rutile type titanium white according to claim 1 or 8, which is characterized in that the surface-active
The mass percentage of agent is 0.1-2%；
Optionally, the surfactant includes cetyltrimethylammonium bromide, neopelex, dodecyl sulphur
At least one of sour sodium and polyethylene glycol.
10. rutile type titanium white made from the preparation method of rutile type titanium white as described in any one of claim 1 to 9
In the application of coating, ink, papermaking, plastic, rubber, chemical fibre and ceramic field.
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| CN111470531A (en) * | 2020-04-07 | 2020-07-31 | 福建富仕新材料有限责任公司 | Rutile type chemical fiber titanium dioxide, preparation method and application |
| CN113353977A (en) * | 2021-07-08 | 2021-09-07 | 福建富仕新材料有限责任公司 | Method for preparing titanium dioxide by using ilmenite |
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Application publication date: 20190628 |