CN116675993A - Preparation method of titanium dioxide modified superfine barium sulfate powder - Google Patents
Preparation method of titanium dioxide modified superfine barium sulfate powder Download PDFInfo
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- CN116675993A CN116675993A CN202310649796.2A CN202310649796A CN116675993A CN 116675993 A CN116675993 A CN 116675993A CN 202310649796 A CN202310649796 A CN 202310649796A CN 116675993 A CN116675993 A CN 116675993A
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- barium sulfate
- titanium dioxide
- sulfate powder
- dioxide modified
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 title claims abstract description 74
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000003607 modifier Substances 0.000 claims abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000011734 sodium Substances 0.000 claims description 13
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- 238000009826 distribution Methods 0.000 claims description 8
- YJHSJERLYWNLQL-UHFFFAOYSA-N 2-hydroxyethyl(dimethyl)azanium;chloride Chemical compound Cl.CN(C)CCO YJHSJERLYWNLQL-UHFFFAOYSA-N 0.000 claims description 6
- 150000002191 fatty alcohols Chemical class 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 3
- 229910052719 titanium Inorganic materials 0.000 claims 3
- 239000010936 titanium Substances 0.000 claims 3
- 239000000463 material Substances 0.000 claims 2
- 238000004064 recycling Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- -1 titanium dioxide modified barium sulfate powder Chemical class 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 239000010428 baryte Substances 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
-
- 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
-
- 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
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/027—Barium sulfates
-
- 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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- 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
- C09C3/063—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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- 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
- C01P2006/12—Surface area
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
-
- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to the field of barium sulfate compounds, and particularly relates to a preparation method of titanium dioxide modified superfine barium sulfate powder. The method comprises the following steps: step 1: adding a composite modifier into barium carbonate slurry, and then adding Na 2 SO 4 Carrying out ultrasonic reaction on the solution; step 2: adding titanyl sulfate, continuing ultrasonic reaction, filtering, washing and drying to obtain the titanium dioxide modified superfine barium sulfate powder. The invention directly coats the titanium dioxide generated by the hydrolysis of the titanyl sulfate on the superfine barium sulfate particles modified by the composite surfactant, has simple process and recycling of resourcesThe method is economical, environment-friendly and free of waste, can effectively control the size and performance of the superfine barium sulfate, and is suitable for industrial production and application.
Description
Technical Field
The invention belongs to the field of barium sulfate compounds, and particularly relates to a preparation method of titanium dioxide modified superfine barium sulfate powder.
Background
Barium sulfate is widely used in the fields of paint, ink, rubber, medicine, plastics, textile, drilling and the like because of the advantages of high whiteness, high chemical stability, abundant resources, low price and the like. In recent years, as the application field continuously upgrades the products, the common barium sulfate has the defects of large particle size, uneven distribution, single surface property, higher impurity content, large batch-to-batch variability and the like, which cannot meet the product requirements. Some superfine functional barium sulfate preparation technologies meeting market requirements are managed and developed, and a high-added-value barium sulfate micropowder production line is established, so that the market competitiveness of barium sulfate in China is improved.
Patent document CN106976900B discloses that barium sulfate is prepared by reacting barite reduced to barium sulfide by calcination with a mirabilite solution from which impurities such as calcium and magnesium have been removed, and the newly generated barium sulfate crystal nucleus is surface-modified by surface modification and dispersing agent sodium stearate, and the barium sulfate particles are further surface-modified by a surface modifier high molecular polymer, so that the barium sulfate particles can be effectively combined with organic high molecules in the powder coating and well dispersed in the coating. The barium sulfate prepared by the method is used for producing the powder coating, and has the advantages of high whiteness, good leveling property, uniform dispersion and the like. Patent document CN103881418B discloses that barium sulfate particles with particle size of 10-1000nm are prepared by taking barium sulfate slurry as a raw material and adding a lubricant, a modifier, a dispersant, a coupling agent, a heat stabilizer, an antioxidant and the like. Patent document CN101418140B discloses that barium sulfate powder suspension obtained by subjecting barium carbonate, sulfuric acid solution and a release agent to a synthesis reaction is subjected to curing, separation, washing, pulping, then surface modification treatment and drying to obtain a finished product. However, the technical process is complex in route, high in equipment investment and not easy for industrialized production. Therefore, development of a technology for preparing ultrafine functional barium sulfate which is simple in process and easy to apply industrially is needed.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the preparation method of the titanium dioxide modified barium sulfate powder, which has the advantages of simple process, resource recycling, no pollution to the environment and easy industrial application.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
a preparation method of titanium dioxide modified superfine barium sulfate powder comprises the following steps:
step 1: adding a composite modifier into the barium carbonate slurry, and then addingNa is introduced into 2 SO 4 Carrying out ultrasonic reaction on the solution;
step 2: adding titanyl sulfate, continuing ultrasonic reaction, filtering, washing and drying to obtain the titanium dioxide modified superfine barium sulfate powder.
The preparation reaction formula of the method is as follows:
BaCO 3 + Na 2 SO 4 ＝ BaSO 4 + Na 2 CO 3 (1)
TiOSO 4 + H 2 O ＝ TiO 2 + H 2 SO 4 (2)
BaCO 3 + H 2 SO 4 ＝ BaSO 4 +H 2 O+CO 2 (3)
Na 2 CO 3 + H 2 SO 4 ＝ Na 2 SO 4 +H 2 O+CO 2 (4)
preferably, in the step 1, the mass concentration of the barium carbonate slurry is 30%.
Preferably, in the step 1, the composite modifier is narrow-distribution fatty alcohol polyoxyethylene ether AEO 3 And the monoalkyl dimethyl hydroxyethyl ammonium chloride is compounded according to the mass ratio of 1:1 to obtain the composite surfactant.
Preferably, in the step 1, the addition amount of the composite modifier is 1 to 5% of the barium carbonate content.
Preferably, in the step 1, the molar ratio of the barium carbonate to the sodium sulfate is 1:1 to 1:1.5.
Preferably, in the step 1, na 2 SO 4 The mass concentration of the solution is 10-30%.
Preferably, in the step 1, the power of the ultrasonic reaction is 1000W-2000W, the reaction temperature is 30-50 ℃, and the reaction time is 2-8 h.
Preferably, in the step 2, the amount of the titanyl sulfate is 0.05 to 0.5 times the amount of the barium carbonate.
Preferably, in the step 2, the power of the ultrasonic reaction is 500-1000w, the reaction temperature is 30-50 ℃ and the reaction time is 0.5-1 h.
Preferably, in the step 2, the particle diameter of the titanium dioxide modified superfine barium sulfate powder is 200 nm-500 nm, the whiteness is 90% -98%, and the specific surface area is 10-40 g/cm 2 。
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the inorganic titanium dioxide is adopted to carry out coating modification on the superfine barium sulfate particles, on one hand, the characteristic of high whiteness of the titanium dioxide is utilized, the problem of low whiteness of the barium sulfate serving as pigment can be solved, and on the other hand, the characteristic of large specific surface area of the titanium dioxide is utilized, the defect of small specific surface area of the superfine barium sulfate is improved, and the defect of small addition amount in the application process is improved.
The invention utilizes titanium oxide sulfate to hydrolyze to produce titanium dioxide which is directly coated on superfine barium sulfate particles modified by the composite surfactant, and the produced byproduct sulfuric acid can convert unreacted barium carbonate into barium sulfate, thereby improving the reaction conversion rate, and simultaneously, the titanium oxide is reacted with byproduct sodium carbonate to produce sodium sulfate which can be used as a reaction raw material for producing the barium sulfate, so that the recycling of resources is achieved. In addition, the modifier compound surfactant added in the preparation process effectively controls the particle size and agglomeration phenomenon of the titanium dioxide modified barium sulfate, and further effectively regulates the particle size distribution of the product. Meanwhile, the conversion rate from barium carbonate to barium sulfate can be effectively improved through the cavitation of ultrasonic waves in the preparation process. The method has the advantages of simple process, resource recycling, economy, environmental protection and no waste, can effectively control the size and the performance of the superfine barium sulfate, and is suitable for industrial production and application.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
30g of barium carbonate is weighed and added into 70ml of distilled water to prepare 30 percent slurry, 0.03g of composite modifier (AEO of narrow-distribution fatty alcohol polyoxyethylene ether) is added into the slurry 3 And monoalkyl dimethyl hydroxyethyl ammonium chloride according to the mass ratio of 1:1), and adding Na with the concentration of 30 percent 2 SO 4 The molar ratio of the solution to the barium carbonate to the sodium sulfate is 1:1, and the solution reacts for 2 hours at 30 ℃ under the ultrasonic action of 1000W of ultrasonic power; then directly adding titanyl sulfate with the quantity of 0.05 times relative to the barium carbonate substance, continuously carrying out ultrasonic reaction for 0.5h with the power of 500w, and concentrating Na by the filtrate 2 SO 4 The recovery rate reaches 90 percent, and the product is filtered, washed and dried at 110 ℃ to obtain the titanium dioxide modified superfine barium sulfate powder with the particle diameter of 500nm, the whiteness Wr of 90 percent and the specific surface area S BET Is 10g/cm 2 。
Example 2
30g of barium carbonate is weighed and added into 70ml of distilled water to prepare 30 percent slurry, and 0.15g of composite modifier (AEO of narrow-distribution fatty alcohol polyoxyethylene ether) is added into the slurry 3 And monoalkyl dimethyl hydroxyethyl ammonium chloride according to the mass ratio of 1:1), and adding 10% concentration Na 2 SO 4 The molar ratio of the solution to the barium carbonate to the sodium sulfate is 1:1.5, and the solution reacts for 8 hours under the ultrasonic action of which the ultrasonic power is 2000w at 50 ℃; then directly adding titanyl sulfate with the quantity of 0.5 times relative to the barium carbonate substance, continuously carrying out ultrasonic reaction for 1h with 1000w power, and concentrating Na in filtrate 2 SO 4 The recovery rate is more than 95 percent, the method can be used for recycling reaction raw material sodium sulfate, and the product is filtered, washed and dried at 110 ℃ to obtain the titanium dioxide modified superfine barium sulfate powder with the particle diameter of 200nm, the whiteness Wr of 98 percent and the specific surface area S BET 40g/cm 2 。
Example 3
30g of barium carbonate is weighed and added into 70ml of distilled water to prepare 30 percent slurry, and 0.1g of composite modifier (AEO of narrow-distribution fatty alcohol polyoxyethylene ether) is added into the slurry 3 And monoalkyl dimethyl hydroxyethyl ammonium chloride according to the mass ratio of 1:1), and adding Na with concentration of 20% 2 SO 4 Solution, barium carbonate andthe molar ratio of sodium sulfate is 1:1.3, and the reaction is carried out for 6 hours at 40 ℃ under the action of ultrasonic waves with the ultrasonic power of 1500W; then directly adding titanyl sulfate with the quantity of 0.2 times relative to the barium carbonate substance, continuously carrying out ultrasonic reaction for 1h with 600w power, and concentrating Na in filtrate 2 SO 4 The recovery rate is over 96 percent, the method can be used for recycling reaction raw material sodium sulfate, and the product is filtered, washed and dried at 110 ℃ to obtain the titanium dioxide modified superfine barium sulfate powder, the particle size is about 400nm, the whiteness Wr is 95 percent, and the specific surface area S BET 20g/cm 2 Left and right.
Example 4
30g of barium carbonate is weighed and added into 70ml of distilled water to prepare 30 percent slurry, and 0.12g of composite modifier (AEO of narrow-distribution fatty alcohol polyoxyethylene ether) is added into the slurry 3 And monoalkyl dimethyl hydroxyethyl ammonium chloride according to the mass ratio of 1:1), and adding Na with the concentration of 15 percent 2 SO 4 The molar ratio of the solution to the barium carbonate to the sodium sulfate is 1:1.2, and the solution reacts for 5 hours at 45 ℃ under the ultrasonic action of which the ultrasonic power is 2000 w; then directly adding titanyl sulfate with the quantity of 0.3 times relative to the barium carbonate substance, continuously carrying out ultrasonic reaction for 1h with 800w power, and concentrating Na in filtrate 2 SO 4 The recovery rate is more than 97 percent, the method can be used for recycling reaction raw material sodium sulfate, and the product is filtered, washed and dried at 110 ℃ to obtain the titanium dioxide modified superfine barium sulfate powder, the particle size is about 300nm, the whiteness Wr is 96 percent, and the specific surface area S BET Is 30g/cm 2 Left and right.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The preparation method of the titanium dioxide modified superfine barium sulfate powder is characterized by comprising the following steps of:
step 1: adding a composite modifier into barium carbonate slurry, and then adding Na 2 SO 4 Carrying out ultrasonic reaction on the solution;
step 2: adding titanyl sulfate, continuing ultrasonic reaction, filtering, washing and drying to obtain the titanium dioxide modified superfine barium sulfate powder.
2. The method for preparing a titanium dioxide-modified ultrafine barium sulfate powder according to claim 1, wherein in the step 1, the mass concentration of the barium carbonate slurry is 30%.
3. The method for preparing titanium dioxide modified superfine barium sulfate powder according to claim 1, wherein in the step 1, the composite modifier is narrow-distribution fatty alcohol polyoxyethylene ether AEO 3 And the monoalkyl dimethyl hydroxyethyl ammonium chloride is compounded according to the mass ratio of 1:1 to obtain the composite surfactant.
4. The method for preparing titanium dioxide modified superfine barium sulfate powder according to claim 1, wherein in the step 1, the addition amount of the composite modifier is 1-5% of the content of barium carbonate.
5. The method for preparing titanium dioxide modified ultrafine barium sulfate powder according to claim 1, wherein in the step 1, the molar ratio of barium carbonate to sodium sulfate is 1:1 to 1:1.5.
6. The method for preparing titanium dioxide-modified ultrafine barium sulfate powder according to claim 1, wherein in the step 1, na 2 SO 4 The mass concentration of the solution is 10-30%.
7. The method for preparing the titanium dioxide modified superfine barium sulfate powder according to claim 1, wherein in the step 1, the power of the ultrasonic reaction is 1000-2000W, the reaction temperature is 30-50 ℃ and the reaction time is 2-8 h.
8. The method for preparing titanium dioxide-modified ultrafine barium sulfate powder according to claim 1, wherein the amount of the titanyl sulfate material in the step 2 is 0.05 to 0.5 times the amount of the barium carbonate material.
9. The method for preparing titanium dioxide modified superfine barium sulfate powder according to claim 1, wherein in the step 2, the power of the ultrasonic reaction is 500-1000w, the reaction temperature is 30-50 ℃ and the reaction time is 0.5-1 h.
10. The method for preparing titanium dioxide modified ultrafine barium sulfate powder according to claim 1, wherein in the step 2, the particle diameter of the titanium dioxide modified ultrafine barium sulfate powder is 200nm to 500nm, the whiteness is 90% to 98%, and the specific surface area is 10g/cm to 40g/cm 2 。
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| CN202310649796.2A Pending CN116675993A (en) | 2023-06-02 | 2023-06-02 | Preparation method of titanium dioxide modified superfine barium sulfate powder |
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