CN107502001A - A kind of method that composite titanium dioxide is prepared using carbide slag - Google Patents

A kind of method that composite titanium dioxide is prepared using carbide slag Download PDF

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Publication number
CN107502001A
CN107502001A CN201710721779.XA CN201710721779A CN107502001A CN 107502001 A CN107502001 A CN 107502001A CN 201710721779 A CN201710721779 A CN 201710721779A CN 107502001 A CN107502001 A CN 107502001A
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China
Prior art keywords
titanium dioxide
carbide slag
composite titanium
calcium
prepared
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CN201710721779.XA
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Chinese (zh)
Inventor
杜高翔
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Shanxi Yiyixing Technology Co Ltd
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Shanxi Yiyixing Technology Co Ltd
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Priority to CN201710721779.XA priority Critical patent/CN107502001A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
    • C09C1/3607—Titanium dioxide
    • C09C1/3653—Treatment with inorganic compounds
    • C09C1/3661—Coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds

Abstract

The invention discloses a kind of method that composite titanium dioxide is prepared using carbide slag.Methods described obtains calcium chloride solution using carbide slag as raw material, by ammonium chloride leaching, adds dispersant, slurry is made in titanium dioxide, and TiO is obtained finally by carbonization2/CaCO3Cladded type composite titanium dioxide.Methods described includes molten calcium, slurrying, is carbonized and four steps of powder processed.The method of the invention is raw material using solid slag carbide slag, both the production cost for preparing composite titanium dioxide had been significantly reduced, again Industrial Solid Waste is reused, obtained composite titanium dioxide possesses the performance similar to titanium dioxide, can be used as the substitute of titanium dioxide.

Description

A kind of method that composite titanium dioxide is prepared using carbide slag
Technical field
The invention belongs to chemical industry solid waste technical field of resource utilization, and in particular to one kind prepares composite titanium dioxide using carbide slag The method of powder.
Background technology
Titanium dioxide, titanium dioxide is commonly called as, is a kind of important industrial chemicals, its physicochemical properties is stable, has simultaneously Excellent optics, electric property and pigment application performance, is widely used in the fields such as coating, chemical fibre, plastics, papermaking, ink. Sulfuric acid process and preparing titanium white through chlorination process powder industrially are used, substantial amounts of poisonous and harmful substance is discharged, significant impact is caused to environment. At present, manufacture composite titanium dioxide is being studied and explored in various countries, to reduce titanium white production cost and Environmental costs.
Composite titanium dioxide is usually using cheap white inorganic powder as kernel, by method physically or chemically, at it Surface coating layer of titanium dioxide particle, formed with core shell structure composite powder material, make composite titanium dioxide possess or The performance of approximate titanium dioxide.
Composite titanium dioxide powder, preparation method thereof one：Nucleome material is reached suitably sized by mechanical lapping, add dioxy Change titanium or TiO 2 precursor, presoma hydrolyze to obtain titanium dioxide fine particles, composite titanium dioxide is finally made.Patent Butyl titanate is added dropwise by the wet grinding of powdered whiting in CN104292886A in process of lapping, hydrolysis generation dioxy Change titanium particulate and be coated on the preferable composite titanium dioxide of the obtained quality of powdered whiting particle surface.Patent CN104387807A is by nothing Suspension is made after machine mineral powder superfine grinding, previously prepared rutile TiO_2 slurries are added dropwise, it is compound that cladded type is made Titanium dioxide.The above-mentioned method high energy consumption for preparing composite titanium dioxide, production cost are higher.
Composite titanium dioxide powder, preparation method thereof two：Calcium carbonate nucleome material is obtained by quicklime slaking, carbonisation, is being carbonized During add titanium dioxide or TiO 2 precursor, presoma and hydrolyze to obtain titanium dioxide fine particles, composite titanium is finally made White powder.Patent CN101302359A quick limes add water to obtain Ca (OH)2Slurries, by TiO2It is beaten and titanium dioxide slurry is made after fine grinding Liquid, at Ca (OH)2Titanium white slurries are added in slurries carbonisation composite titanium dioxide is made.Patent CN103194098A is then light The carbonation stage of matter calcium carbonate production process adds metatitanic acid and is made as titanium source covering.The above method in preparation process with Quick lime adds water digestion to be carbonized to obtain CaCO again3, cost of material is big, and production process need to be equipped with special digestion facility, expends Equipment and management cost it is larger.
Carbide slag is caused trade waste during calcium carbide and water reaction generation acetylene gas, and main component is hydrogen Calcium oxide, contain the impurity such as a small amount of silicon, iron, aluminium, magnesium.Carbide slag bulk deposition not only land occupation, and seriously pollution week Surrounding environment.Composite titanium dioxide is prepared using carbide slag, the production on the one hand reducing carbide slag and titanium dioxide is dirty to caused by environment Dye, a new approach on the other hand is have found to explore the utilization of carbide slag solid waste and preparing composite titanium dioxide, substantially reduces titanium White powder prepares cost, has great research and actual application value.
The content of the invention
In order to solve the problems such as high cost existing for existing titanium white powder, preparation method thereof, high energy consumption, the present invention provides a kind of The method that composite titanium dioxide is prepared using carbide slag.Methods described passes through the leaching of ammonium chloride using Industrial Solid Waste carbide slag as raw material Obtain calcium chloride solution, first and titanium dioxide mixed pulp, then the obtained composite titanium dioxide that is carbonized.Compared with the conventional method, it is described Method has relatively low energy consumption and production cost, Industrial Solid Waste carbide slag is utilized effectively, more energy-conserving and environment-protective, is advantageous to Industrialized production.
To realize above-mentioned target, the present invention uses following technical scheme：
A kind of method that composite titanium dioxide is prepared using carbide slag, methods described pass through ammonium chloride using carbide slag as raw material Leaching obtains calcium chloride solution, adds dispersant, slurry is made in titanium dioxide, and TiO is obtained finally by carbonization2/CaCO3Bag Cover type composite titanium dioxide.
Methods described has claimed below to raw material selection：
1) carbide slag, Industrial Solid Waste, Ca (OH)2Content 85%~95%, the mesh of fineness 100~2500；
2) titanium dioxide, technical grade, TiO2Content is more than 93%；
3) ammonium chloride, technical grade；
4) hydrogen peroxide, technical grade；
5) carbon dioxide, partial pressure 10%~100%.
It the described method comprises the following steps：
1) molten calcium：Carbide slag, ammonium chloride, hydrogen peroxide are mixed with water, 20~30min of stirring reaction so that calcium ion base This dissolution, impurity are removed with precipitation form, raw material proportioning requirement：Carbide slag and ammonium chloride mass ratio are 1:0.5~2, hydrogen peroxide Quality is the 1%~5% of carbide slag quality, and water is 6~10 with carbide slag mass ratio:1；
2) slurrying：The slurry by filtration that step 1) is obtained, the calcium chloride solution clarified, added into filtrate and account for calcium carbide The dispersant of slag amount 0.5%~5%, then titanium dioxide is added in calcium chloride solution, then gained mixture is put into In agitator tank, slurry is stirred into, is converted with calcium in carbide slag, titanium dioxide quality：Calcium carbonate quality=1:1~3；
3) it is carbonized：The CO that flow velocity is 1~1.5L/min is passed through in the slurry obtained to step 2)2Gas be carbonized instead Should, CO2Partial pressure 10%~100%, when the pH value of solution is in 6.0-8.0 stop be passed through gas, now calcium chloride transformation into Calcium carbonate, and coated by titanium dioxide is in calcium carbonate surface；
4) powder processed：By the filtering of product that step 3) obtains, washing, dry, break up and obtain that there is the compound of core shell structure Titanium dioxide.
Preferably, the dispersant is Sodium Polyacrylate.
Preferably, the CO of the carbonization2Gas can use close on factory smoke.
By the method for the invention, finally the composition of obtained composite titanium dioxide and composition are (mass percent)：Carbonic acid Calcium 50%-75%, titanium dioxide 25%-50%.
The advantages of the present invention are：
1) with carbide slag raw material, both solved the problems, such as the recycling of Industrial Solid Waste carbide slag, and alleviated environmental pressure, protected again The cheap of raw material and abundant supply have been demonstrate,proved, has reduced the production cost of composite titanium dioxide；
2) flue gas for closing on factory can be utilized to replace the CO of carbonization2Gas, more energy-conserving and environment-protective, be advantageous to industrialize Production.
Embodiment
Embodiment 1
1) molten calcium：100g carbide slags, 100g ammonium chlorides, 800mL water, the mixing of 3g hydrogen peroxide are weighed, is sufficiently stirred, reacts After 20min, product is filtered, the calcium chloride solution clarified；
2) slurrying：1g Sodium Polyacrylates are added into filtrate, is sufficiently stirred, adds 67.5g titanium dioxide, be put into stirring Slurry is stirred into tank；
3) it is carbonized：The CO that partial pressure is 50% is passed through into above-mentioned slurry while stirring2Gas, stable flow velocity 1.5L/min, Stop reaction when slurry pH is 7.0；
4) powder processed：By above-mentioned product filtering, washing, dry, break up after obtain composite titanium dioxide.
Embodiment 2
1) molten calcium：100g carbide slags, 50g ammonium chlorides, 600mL water, the mixing of 1g hydrogen peroxide are weighed, is sufficiently stirred, reacts After 20min, product is filtered, the calcium chloride solution clarified；
2) slurrying：0.5g Sodium Polyacrylates are added into filtrate, is sufficiently stirred, adds 50g titanium dioxide, be put into stirring Slurry is stirred into tank；
3) it is carbonized：The CO that partial pressure is 10% is passed through into above-mentioned slurry while stirring2Gas, stable flow velocity 1L/min, is treated Stop reaction when slurry pH is 6.0；
4) powder processed：By above-mentioned product filtering, washing, dry, break up after obtain composite titanium dioxide.
Embodiment 3
1) molten calcium：100g carbide slags, 200g ammonium chlorides, 1000mL water, the mixing of 5g hydrogen peroxide are weighed, is sufficiently stirred, reacts After 30min, product is filtered, the calcium chloride solution clarified；
2) slurrying：5g Sodium Polyacrylates are added into filtrate, is sufficiently stirred, is added 16g titanium dioxide, be put into agitator tank In stir into slurry；
3) it is carbonized：The CO that partial pressure is 100% is passed through into above-mentioned slurry while stirring2Gas, stable flow velocity 1.3L/min, Stop reaction when slurry pH is 8.0；
4) powder processed：By above-mentioned product filtering, washing, dry, break up after obtain composite titanium dioxide.
Finally it should be noted that：Obviously, above-described embodiment is only intended to clearly illustrate example of the present invention, and simultaneously The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description Go out other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn Among the obvious changes or variations of stretching is still in protection scope of the present invention.

Claims (6)

  1. A kind of 1. method that composite titanium dioxide is prepared using carbide slag, it is characterised in that：Methods described is led to using carbide slag as raw material Superchlorination ammonium leaches to obtain calcium chloride solution, adds dispersant, slurry is made in titanium dioxide, is obtained finally by carbonization TiO2/CaCO3Cladded type composite titanium dioxide.
  2. A kind of 2. method that composite titanium dioxide is prepared using carbide slag as claimed in claim 1, it is characterised in that methods described Have to raw material claimed below：
    1) carbide slag, Industrial Solid Waste, Ca (OH)2Content 85%~95%, the mesh of fineness 100~2500；
    2) titanium dioxide, technical grade, TiO2Content is more than 93%；
    3) ammonium chloride, technical grade；
    4) hydrogen peroxide, technical grade；
    5) carbon dioxide, partial pressure 10%~100%.
  3. A kind of 3. method that composite titanium dioxide is prepared using carbide slag as claimed in claim 1, it is characterised in that methods described Comprise the following steps：
    1) molten calcium：Carbide slag, ammonium chloride, hydrogen peroxide are mixed with water, 20~30min of stirring reaction so that calcium ion is substantially molten Go out, impurity is removed with precipitation form, raw material proportioning requirement：Carbide slag and ammonium chloride mass ratio are 1:0.5~2, dioxygen water quality It is the 1%~5% of carbide slag quality, water is 6~10 with carbide slag mass ratio:1；
    2) slurrying：The slurry by filtration that step 1) is obtained, the calcium chloride solution clarified, added into filtrate and account for calcium carbide slag The dispersant of amount 0.5%~5%, then titanium dioxide is added in calcium chloride solution, gained mixture is then put into stirring In tank, slurry is stirred into, is converted with calcium in carbide slag, titanium dioxide quality：Calcium carbonate quality=1:1~3；
    3) it is carbonized：The CO that flow velocity is 1~1.5L/min is passed through in the slurry obtained to step 2)2Gas carries out carburizing reagent, CO2 Partial pressure 10%~100%, stop being passed through gas when the pH value of solution is in 6.0-8.0, now calcium chloride transformation is into calcium carbonate, And coated by titanium dioxide is in calcium carbonate surface；
    4) powder processed：The product that step 3) obtains is filtered, washed, is dried, breaks up the composite titanium dioxide for obtaining that there is core shell structure Powder.
  4. A kind of 4. method that composite titanium dioxide is prepared using carbide slag as described in claim 1,2,3, it is characterised in that：It is described Dispersant is Sodium Polyacrylate.
  5. A kind of 5. method that composite titanium dioxide is prepared using carbide slag as described in claim 1,2,3, it is characterised in that：It is described The CO of carbonization2Gas can use close on factory smoke.
  6. 6. a kind of method that composite titanium dioxide is prepared using carbide slag as described in claim 1,2,3, it is characterised in that pass through The composition of composite titanium dioxide made from methods described is with mass percent：Calcium carbonate 50%-75%, titanium dioxide 25%- 50%.
CN201710721779.XA 2017-08-22 2017-08-22 A kind of method that composite titanium dioxide is prepared using carbide slag Pending CN107502001A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115109437A (en) * 2022-07-12 2022-09-27 龙佰禄丰钛业有限公司 Preparation method of composite titanium dioxide

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101302359A (en) * 2008-06-30 2008-11-12 攀枝花学院 Composite titanium pigment and preparation thereof
CN101993104A (en) * 2009-08-21 2011-03-30 北京紫光英力化工技术有限公司 Novel method for producing superfine calcium carbonate by using carbide slag as raw material
CN104229852A (en) * 2014-09-12 2014-12-24 中国科学院过程工程研究所 Surface modification method for fine calcium carbonate prepared by utilizing calcium carbide slag
CN105217671A (en) * 2014-06-17 2016-01-06 阜阳师范学院 A kind of method utilizing carbide slag to prepare light calcium carbonate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101302359A (en) * 2008-06-30 2008-11-12 攀枝花学院 Composite titanium pigment and preparation thereof
CN101993104A (en) * 2009-08-21 2011-03-30 北京紫光英力化工技术有限公司 Novel method for producing superfine calcium carbonate by using carbide slag as raw material
CN105217671A (en) * 2014-06-17 2016-01-06 阜阳师范学院 A kind of method utilizing carbide slag to prepare light calcium carbonate
CN104229852A (en) * 2014-09-12 2014-12-24 中国科学院过程工程研究所 Surface modification method for fine calcium carbonate prepared by utilizing calcium carbide slag

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115109437A (en) * 2022-07-12 2022-09-27 龙佰禄丰钛业有限公司 Preparation method of composite titanium dioxide

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Application publication date: 20171222