CN106221297B - The method for improving the surface organic process of titanium dioxide dispersibility - Google Patents
The method for improving the surface organic process of titanium dioxide dispersibility Download PDFInfo
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- CN106221297B CN106221297B CN201610586610.3A CN201610586610A CN106221297B CN 106221297 B CN106221297 B CN 106221297B CN 201610586610 A CN201610586610 A CN 201610586610A CN 106221297 B CN106221297 B CN 106221297B
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- 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
- C09C1/3669—Treatment with low-molecular organic compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3684—Treatment with organo-silicon compounds
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- 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
- C09C1/3692—Combinations of treatments provided for in groups C09C1/3615 - C09C1/3684
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- 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
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- 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
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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Abstract
The present invention relates to a kind of methods of surface organic process, more particularly to the method for the surface organic process for the performance for improving rutile type titanium white, belong to chemical field.The defects of to overcome existing rutile type titanium white surface organic process method, polymolecularity and the rutile type titanium white of high aqueous covering power are prepared, the method that the present invention improves the surface organic process of titanium dioxide dispersibility includes the following steps：A, the titanium dioxide after inorganic coating is spent into ionized water and is prepared into titanium dioxide suspension；B, by suspension insulated and stirred；C, aqueous citric acid solution is added dropwise, continues insulated and stirred；D, organic agent is added dropwise, continues insulated and stirred；E, suspension is dried, and carries out air-flow crushing.There is the inaccessiable good characteristic of other methods, especially water dispersible and aqueous covering power using the rutile titanium white that this method obtains, there is good application and promotion prospect.
Description
Technical field
The present invention relates to a kind of method of surface organic process, more particularly to the performance for improving rutile type titanium white
The method of surface organic process, belongs to chemical field.
Background technology
Titanium dioxide is important inorganic functional material, because of its unique physics, chemical property, is widely used in painting
The organic chemical industries such as material, plastics, papermaking, ink field.Surface organic process can improve titanium dioxide and resin and organic solvent
Compatibility, so as to improve the application performance of titanium dioxide.
It is reported according to current pertinent literature, organic agent adds in dry and air-flow crushing two procedures in industrial production
Add, adsorbed in a manner of physically or chemically on titanium dioxide surface, organic process effect is by detecting dispersibility, the oil suction of titanium dioxide
The application performances such as the pigment performances such as amount, brightness index and covering power, glossiness indexs characterizes.Organic process influential effect is to titanium
The dispersibility of white powder, the indexs such as the stability and covering power of oil absorption.
In the rutile type titanium white surface organic process technology being related to, there has been no improve titanium white by pretreatment mode
The organic process technology and methods of powder surface organic process effect.
Invention content
Present invention solves the technical problem that be the defects of overcoming existing rutile type titanium white surface organic process method,
Prepare polymolecularity and the rutile type titanium white of high aqueous covering power.
In order to solve the above-mentioned technical problem, the method that the present invention improves the surface organic process of titanium dioxide dispersibility is included such as
Lower step：
A, the titanium dioxide after inorganic coating is spent into ionized water and is prepared into titanium dioxide suspension；
B, suspension is heated to 55~65 DEG C, insulated and stirred；
C, aqueous citric acid solution is added dropwise, continues insulated and stirred, wherein citric acid dosage is the 0.10% of titanium dioxide solid content
~0.20%；
D, organic agent is added dropwise, continues insulated and stirred；
E, suspension is dried, and crushed.
Preferably, temperature step b, kept the temperature described in c and d is 60 DEG C.
Further, the suspension concentration of the titanium dioxide described in step a is 180~220g/L, preferably 200g/L.
Further, the time of the stirring described in step b is 20~40min, preferably 30min.
Further, a concentration of 40~60g/L of aqueous citric acid solution described in step c.
Further, 20~40min of mixing time described in step c.
Further, the organic agent described in step d can be silicone oil emulsion, it is Modified silicon oil emulsion, silane coupled
At least one of agent and trimethylolpropane, wherein, organic agent dosage for titanium dioxide solid content 0.50%~
1.00%.
Wherein, citric acid dosage: organic agent dosage=1: 5.
Further, 20~40min of mixing time described in step d.
Further, the suspension drying temperature described in step e is 105~120 DEG C, suspension drying time for 36~
48h。
Compared with existing titanium dioxide organic process technology, the present invention pre-processes titanium dioxide using citric acid, passes through
Chemical action, making organic agent, more stably overseas Chinese federation on titanium dioxide surface, effectively increases organic agent in titanium dioxide table
Face adsorption rate and absorption uniformity；Under the premise of citric acid dosage is controlled, the performance of product can be significantly improved, including dispersion
Property, covering power and mobility etc..There is the inaccessiable good characteristic of other methods using the rutile titanium white that this method obtains,
Especially water dispersible and aqueous covering power have good application and promotion prospect.
Specific embodiment
The method that the present invention improves the surface organic process of titanium dioxide dispersibility includes the following steps：
A, the titanium dioxide after inorganic coating is spent into ionized water and is prepared into titanium dioxide suspension；
B, suspension is heated to 55~65 DEG C, insulated and stirred；
C, aqueous citric acid solution is added dropwise, continues insulated and stirred, wherein citric acid dosage is the 0.10% of titanium dioxide solid content
~0.20%；
D, organic agent is added dropwise, continues insulated and stirred；
E, suspension is dried, and crushed.
Wherein, when temperature step b, kept the temperature described in c and d is 60 DEG C, effect is best.
The suspension concentration of titanium dioxide described in step a is unsuitable excessively high, also unsuitable relatively low, the suspension concentration of titanium dioxide
It is advisable in 180~220g/L, the suspension concentration 200g/L effects of wherein titanium dioxide are optimal.
The time of stirring described in step b is uneven for too short titanium white powder particles, and the long production efficiency of mixing time is not
Height, mixing time are advisable in 20~40min, and mixing time 30min is best.
Further, a concentration of 40~60g/L of aqueous citric acid solution described in step c.
Further, 20~40min of mixing time described in step c.
Further, the organic agent described in step d can be silicone oil emulsion, it is Modified silicon oil emulsion, silane coupled
At least one of agent and trimethylolpropane, wherein preferably, organic agent dosage is titanium dioxide solid content
0.50%~1.00%.
Wherein, citric acid dosage: organic agent dosage=1: 5.
Further, 20~40min of mixing time described in step d.
Wherein, the suspension drying temperature described in step e is 105~120 DEG C, and suspension drying time is 36~48h,
Wherein suspension drying temperature must not be higher than 120 DEG C；The drying time of suspension can be adjusted with drying temperature, temperature Gao Ze
Drying time is few, and temperature is low, then drying time is long, for example, by using 105 DEG C of drying temperature, then drying time 48h, if using
120 DEG C of drying temperature, then drying time 36h.
The specific embodiment of the present invention is further described with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
The titanium dioxide after 200g inorganic coatings is taken, is beaten with deionized water, a concentration of 200g/ of the Titanium dioxide slurry after mashing
L, Titanium dioxide slurry heating water bath are sufficiently stirred 30min to 60 DEG C；
Above-mentioned slurry is added in the citric acid solution 4ml of a concentration of 50g/L, then is sufficiently stirred 30min, then by titanium dioxide
Solid content meter adds in 0.50% silicone oil emulsion, is sufficiently stirred 30min；
By 120 DEG C of drying 36h of slurry, air-flow crushing is carried out, obtains titanium dioxide product.
Detection obtains：The titanium dioxide oil-dispersing property of embodiment 1 is 6.50,44 μm of water dispersible, and aqueous covering power is
89.25%.
Embodiment 2
The titanium dioxide after 200g inorganic coatings is taken, is beaten with deionized water, a concentration of 200g/ of the Titanium dioxide slurry after mashing
L, Titanium dioxide slurry heating water bath are sufficiently stirred 30min to 60 DEG C；
Above-mentioned slurry is added in the citric acid solution 8ml of a concentration of 50g/L, then is sufficiently stirred 30min, then by titanium dioxide
Solid content meter adds in 1.00% hydroxyl modification organic silicon emulsion, is sufficiently stirred 30min；
By 105 DEG C of drying 48h of slurry, air-flow crushing is carried out, obtains titanium dioxide product.
Detection obtains：Titanium dioxide oil-dispersing property is 6.75,30 μm of water dispersible, and aqueous covering power is 92.88%.
Embodiment 3
The titanium dioxide after 200g inorganic coatings is taken, is beaten with deionized water, a concentration of 220g/ of the Titanium dioxide slurry after mashing
L, Titanium dioxide slurry heating water bath are sufficiently stirred 20min to 65 DEG C；
The citric acid solution 4ml of a concentration of 60g/L will be added in above-mentioned slurry, then be sufficiently stirred 20min, then by titanium white
Powder solid content meter adds in 0.60% organic silicon modified by polyether lotion, is sufficiently stirred 20min；
By 105 DEG C of drying 48h of slurry, air-flow crushing is carried out, obtains titanium dioxide product.
Detection obtains：Titanium dioxide oil-dispersing property is 6.50,25 μm of water dispersible, and aqueous covering power is 91.55%.
Embodiment 4
The titanium dioxide after 200g inorganic coatings is taken, is beaten with deionized water, a concentration of 180g/ of the Titanium dioxide slurry after mashing
L, Titanium dioxide slurry heating water bath are sufficiently stirred 40min to 55 DEG C；
The citric acid solution 7.5ml of a concentration of 40g/L will be added in above-mentioned slurry, then be sufficiently stirred 40min, then by titanium
White powder solid content meter adds in 0.75% hydroxyl modification organic silicon emulsion, is sufficiently stirred 40min；
By 105 DEG C of drying 48h of slurry, air-flow crushing is carried out, obtains titanium dioxide product.
Detection obtains：Titanium dioxide oil-dispersing property is 6.50,35 μm of water dispersible, and aqueous covering power is 91.02%.
Comparative example 1
Comparative example 1 is the parallel test of embodiment 1, is added without from comparative example 1 unlike embodiment 1 is unique a concentration of
The citric acid solution 4ml of 50g/L, the step of being sufficiently stirred 30min.
Detection obtains：The titanium dioxide oil-dispersing property 6.00 of comparative example 1,54 μm of water dispersible, aqueous covering power are
85.05%.
Comparative example 2
Comparative example 2 is the parallel test of embodiment 2, is added without from comparative example 2 unlike embodiment 2 is unique a concentration of
The citric acid solution 8ml of 50g/L, then the step of be sufficiently stirred 30min.
Detection obtains：The titanium dioxide oil-dispersing property 6.25 of comparative example 2,44 μm of water dispersible, aqueous covering power are
88.79%.
As it can be seen that titanium dioxide moisture made from the method for the surface organic process using the present invention for improving titanium dioxide dispersibility
It dissipates property and aqueous covering power is very good, there is good application and promotion prospect.
Claims (33)
1. improve the method for the surface organic process of titanium dioxide dispersibility, it is characterised in that include the following steps：
A, the titanium dioxide after inorganic coating is spent into ionized water and is prepared into titanium dioxide suspension；
B, suspension is heated to 55~65 DEG C, insulated and stirred；
C, be added dropwise aqueous citric acid solution, continue insulated and stirred, wherein citric acid dosage for titanium dioxide solid content 0.10%~
0.20%；
D, organic agent is added dropwise, continues insulated and stirred；
E, suspension is dried, and crushed；
Organic agent described in step d is silicone oil emulsion, at least one of Modified silicon oil emulsion, wherein, organic process
Agent dosage is the 0.50%~1.00% of titanium dioxide solid content.
2. the method for the surface organic process according to claim 1 for improving titanium dioxide dispersibility, it is characterised in that step
B, the temperature 60 C kept the temperature described in c and d.
3. the method for the surface organic process according to claim 1 or 2 for improving titanium dioxide dispersibility, it is characterised in that step
The suspension concentration of titanium dioxide described in rapid a is 180~220g/L.
4. the method for the surface organic process according to claim 3 for improving titanium dioxide dispersibility, it is characterised in that step a
Described in titanium dioxide suspension concentration be 200g/L.
5. the method for the surface organic process of titanium dioxide dispersibility is improved according to 1,2,4 any one of them of claim, it is special
Sign is that the time of the stirring described in step b is 20~40min.
6. the method for the surface organic process according to claim 3 for improving titanium dioxide dispersibility, it is characterised in that step b
Described in stirring time be 20~40min.
7. the method for the surface organic process according to claim 5 for improving titanium dioxide dispersibility, it is characterised in that step b
Described in stirring time be 30min.
8. the method for the surface organic process according to claim 6 for improving titanium dioxide dispersibility, it is characterised in that step b
Described in stirring time be 30min.
9. the method for the surface organic process of titanium dioxide dispersibility is improved according to 1,2,4,6~8 any one of them of claim,
It is characterized in that a concentration of 40~60g/L of aqueous citric acid solution described in step c.
10. the method for the surface organic process according to claim 3 for improving titanium dioxide dispersibility, it is characterised in that step
A concentration of 40~60g/L of aqueous citric acid solution described in c.
11. the method for the surface organic process according to claim 5 for improving titanium dioxide dispersibility, it is characterised in that step
A concentration of 40~60g/L of aqueous citric acid solution described in c.
12. the organic place in surface of titanium dioxide dispersibility is improved according to 1,2,4,6~8,10~11 any one of them of claim
The method of reason, it is characterised in that citric acid quality: organic agent quality=1: 5.
13. the method for the surface organic process according to claim 3 for improving titanium dioxide dispersibility, it is characterised in that lemon
Sour quality: organic agent quality=1: 5.
14. the method for the surface organic process according to claim 5 for improving titanium dioxide dispersibility, it is characterised in that lemon
Sour quality: organic agent quality=1: 5.
15. the method for the surface organic process according to claim 9 for improving titanium dioxide dispersibility, it is characterised in that lemon
Sour quality: organic agent quality=1: 5.
16. the surface of titanium dioxide dispersibility is improved according to 1,2,4,6~8,10~11,13~15 any one of them of claim
The method of organic process, it is characterised in that 20~40min of mixing time described in step c.
17. the method for the surface organic process according to claim 3 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in c.
18. the method for the surface organic process according to claim 5 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in c.
19. the method for the surface organic process according to claim 9 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in c.
20. the method for the surface organic process according to claim 12 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in rapid c.
21. titanium dioxide dispersion is improved according to 1,2,4,6~8,10~11,13~15,17~20 any one of them of claim
The method of the surface organic process of property, it is characterised in that 20~40min of mixing time described in step d.
22. the method for the surface organic process according to claim 3 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in d.
23. the method for the surface organic process according to claim 5 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in d.
24. the method for the surface organic process according to claim 9 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in d.
25. the method for the surface organic process according to claim 12 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in rapid d.
26. the method for the surface organic process according to claim 16 for improving titanium dioxide dispersibility, it is characterised in that step
20~40min of mixing time described in rapid d.
27. titanium white is improved according to 1,2,4,6~8,10~11,13~15,17~20,22~26 any one of them of claim
The method of the surface organic process of powder dispersibility, it is characterised in that the suspension drying temperature described in step e is 105~120
DEG C, suspension drying time is 36~48h.
28. the method for the surface organic process according to claim 3 for improving titanium dioxide dispersibility, it is characterised in that step
Suspension drying temperature described in e is 105~120 DEG C, and suspension drying time is 36~48h.
29. the method for the surface organic process according to claim 5 for improving titanium dioxide dispersibility, it is characterised in that step
Suspension drying temperature described in e is 105~120 DEG C, and suspension drying time is 36~48h.
30. the method for the surface organic process according to claim 9 for improving titanium dioxide dispersibility, it is characterised in that step
Suspension drying temperature described in e is 105~120 DEG C, and suspension drying time is 36~48h.
31. the method for the surface organic process according to claim 12 for improving titanium dioxide dispersibility, it is characterised in that step
Suspension drying temperature described in rapid e is 105~120 DEG C, and suspension drying time is 36~48h.
32. the method for the surface organic process according to claim 16 for improving titanium dioxide dispersibility, it is characterised in that step
Suspension drying temperature described in rapid e is 105~120 DEG C, and suspension drying time is 36~48h.
33. the method for the surface organic process according to claim 21 for improving titanium dioxide dispersibility, it is characterised in that step
Suspension drying temperature described in rapid e is 105~120 DEG C, and suspension drying time is 36~48h.
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| CN107805410B (en) * | 2017-11-24 | 2020-07-07 | 中信钛业股份有限公司 | Titanium dioxide production method for improving dispersibility in resin system |
| CN108384285A (en) * | 2018-03-08 | 2018-08-10 | 四川龙蟒钛业股份有限公司 | A kind of preparation method of high dispersive titanium dioxide |
| CN108587243A (en) * | 2018-03-08 | 2018-09-28 | 四川龙蟒钛业股份有限公司 | A kind of production method of high heap density color masterbatch grade titanium dioxide |
| CN108587247A (en) * | 2018-07-10 | 2018-09-28 | 四川龙蟒钛业股份有限公司 | A kind of production method of low VOC titanium dioxides |
| CN109438990B (en) * | 2018-11-16 | 2021-02-02 | 山东道安新材料有限公司 | Composite silicone oil emulsion and preparation method thereof |
| CN110452560A (en) * | 2019-08-28 | 2019-11-15 | 四川龙蟒钛业股份有限公司 | A kind of production method of the high heap density color masterbatch grade titanium dioxide of high-temperature resistant |
| CN113387383B (en) * | 2021-05-24 | 2022-10-28 | 龙佰四川钛业有限公司 | Production method of high-fluidity titanium dioxide flash drying material |
| CN113637354B (en) * | 2021-07-30 | 2023-05-23 | 中建材（合肥）新能源有限公司 | High-reflectivity water-based ink for photovoltaic module backboard glass |
| CN115124862B (en) * | 2022-07-12 | 2023-11-10 | 攀钢集团重庆钒钛科技有限公司 | Modified titanium dioxide and preparation method thereof |
| CN115850998A (en) * | 2022-11-30 | 2023-03-28 | 攀钢集团研究院有限公司 | Method for improving brightness of titanium dioxide |
| CN115850999A (en) * | 2022-11-30 | 2023-03-28 | 攀钢集团研究院有限公司 | Preparation method of titanium dioxide for high-gloss high-dispersion ink |
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| CN1858309A (en) * | 2006-01-10 | 2006-11-08 | 上海千泰高科技发展有限公司 | Titanium white for dry acrylic spinning delustering its preparing method |
| CN102993786A (en) * | 2012-08-31 | 2013-03-27 | 道奇威（成都）科技有限公司 | Organic surface modification method for improving water dispersion stability of rutile titanium dioxide |
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