CN107500347A - A kind of method for controlling decorating base paper titanium dioxide particle diameter - Google Patents
A kind of method for controlling decorating base paper titanium dioxide particle diameter Download PDFInfo
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- CN107500347A CN107500347A CN201710790698.5A CN201710790698A CN107500347A CN 107500347 A CN107500347 A CN 107500347A CN 201710790698 A CN201710790698 A CN 201710790698A CN 107500347 A CN107500347 A CN 107500347A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
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Abstract
A kind of method for controlling decorating base paper titanium dioxide particle diameter, belongs to the technical field of decorating base paper titanium dioxide, by controlling hydrolyzing process, comprises the following steps：A, 96 98 DEG C are preheating to from titanium sulfate liquid, it is standby；Desalted water is preheated to boiling, it is standby；B, the desalted water for being preheated to boiling is charged first in hydrolysis reactor, stirred, then add the titanium sulfate liquid of preheating, after titanium sulfate liquid adds, stirring, be heated to micro-boiling；C, treat that step B percent hydrolysis up to 50 65%, stops stirring, stops heating, cured；D, after curing, it is stirred again, is heated to micro-boiling 160 180min are hydrolyzed；E, boiling desalted water is added, controls total titanium concentration TiO in slurry2160 180g/L, micro-boiling is kept, hydrolyze 50 60min.The inventive method makes titanium sulfate liquid pyrohydrolysis technology meet that decorating base paper requirement is implemented, and water and titanium dioxide uniform particle sizes, meets the technology for hydrolyzing that the Particle size requirements of decorating base paper titanium dioxide specially design.
Description
Technical field
The invention belongs to the technical field of decorating base paper titanium dioxide, is related to the research of decorating base paper titanium dioxide particle diameter, specifically
It is related to a kind of method for controlling decorating base paper titanium dioxide particle diameter.The inventive method makes titanium sulfate liquid pyrohydrolysis technology meet that decoration is former
Paper requires to implement, and water and titanium dioxide uniform particle sizes, the hydrolysis specially designed for the Particle size requirements of decorating base paper titanium dioxide
Technology.By from technology for hydrolyzing starting with, make to reach the advantage of chloridising with titanium dioxide particle diameter prepared by sulfuric acid process, and then make preparation
Decorating base paper either covering power, whiteness, gloss all compared favourably with Titanium Dioxide Produced by Chloride Procedure.
Background technology
Decorating base paper is that one kind is formed using the color stuffing such as high-quality wood pulp and titanium dioxide (accounting for 30% or so) as Raw material processing
Industrial special type paper.Titanium dioxide plays decisive work to performances such as the covering power of decorating base paper, whiteness, gloss, weatherability, smoothnesses
With.Requirement of the high-grade decorating base paper to titanium dioxide：(1) whiteness height, good luster；(2) covering power is high；(3) good dispersion；(4) weatherability
It is good.One key factor of these characteristics of titanium dioxide is exactly the particle diameter of titanium dioxide, and decorating base paper will to the particle diameter of titanium dioxide
Ask different from fields such as coating, plastics.
The titanium white production method of decorating base paper has two kinds, and one kind is sulfuric acid process, and one kind is chloridising.Global sulfuric acid process production
Can about 50%, production capacity account for global half China based on sulfuric acid process, account for more than 95% production capacity.
Titanium sulfate liquid pyrohydrolysis is sulfuric acid method titanium pigment production center link, the major control target of pyrohydrolysis be exactly water and
The particle diameter of titanium dioxide.The particle diameter of hydrated titanium dioxide determines the operating condition of subsequent handling and the optical property of product, its
It is middle influence it is maximum be titanium dioxide covering power, be mainly reflected in the opacity of decorating base paper.
Sulfuric acid method titanium pigment production technology foreign countries are molded in the seventies in last century, and new technical research there is no report
Road.Chinese titanium dioxide industry is risen to be rapidly developed in the beginning of the nineties in last century, this century, but technical research is seldom, mainly
Still continue to use the technology before East European countries seventies in last century, some enterprises by exchange study world sulfuric acid process some zero
The advanced experience of star, industry homogeneity is very serious, and the control to titanium dioxide particle diameter is paid attention to not enough, causing later stage application effect
Be not as good as Titanium Dioxide Produced by Chloride Procedure effect.
The content of the invention
Applied defect of the main object of the present invention aiming at current sulfuric acid method titanium pigment in decorating base paper, from titanium white
The hydrolysis process technology of powder is started with, there is provided a kind of control method for meeting decorating base paper titanium dioxide particle diameter particular/special requirement.By excellent
Different technology for hydrolyzing reaches the effect of control decorating base paper titanium dioxide particle diameter, carrys out table with decorating base paper impregnation laminated paper opacity
Levy the quality of titanium dioxide particle diameter.
The present invention is to realize that the technical scheme that its purpose uses is：
A kind of method for controlling decorating base paper titanium dioxide particle diameter, by controlling hydrolyzing process, comprises the following steps：
A, from total titanium concentration TiO2215-235g/L、Ti3+Concentration 1.0-3.0g/L, sour ratio 1.7-2.0, Fe2+/TiO2
0.27-0.31, stability >=500ml, solid formation≤30mg/L titanium sulfate liquid, are preheating to 96-98 DEG C, standby；By desalted water
Boiling is preheated to, it is standby；
B, the desalted water for being preheated to boiling is charged first in hydrolysis reactor, stirred, then add the titanium sulfate of preheating
Liquid, the volume ratio for controlling desalted water and titanium sulfate liquid is 20-25%, after titanium sulfate liquid adds, stirring, is heated to micro-boiling
Rise；
C, treat that step B percent hydrolysis reaches 50-65%, stop stirring, stop heating, cured；
D, after curing, it is stirred again, is heated to micro-boiling 160-180min is hydrolyzed；
E, boiling desalted water is added, controls total titanium concentration TiO in slurry2160-180g/L, micro-boiling is kept, hydrolyze 50-
60min。
The temperature of micro-boiling is 112-118 DEG C in step B, and it is 18-20min to control the heat temperature raising time.
The temperature of curing is that the time of curing is 20-30min.
The temperature of micro-boiling is 114-118 DEG C in step D, and it is 18-20min to control the heat temperature raising time.
The temperature of micro-boiling is 108-112 DEG C in step E.
Total titanium concentration TiO is selected in step A2225-235g/L、Ti3+Concentration 1.0-3.0g/L, sour ratio 1.7-1.85,
Fe2+/TiO20.27-0.29, stability >=500ml, solid formation≤30mg/L titanium sulfate liquid.
In step E, boiling desalted water is added, controls total titanium concentration TiO in slurry2160-170g/L。
The beneficial effects of the invention are as follows：
The hydrolysate metatitanic acid particle that the control of method for hydrolysis of the present invention makes to obtain is uniform in size on the whole, round and smooth, and one
Good, the percent hydrolysis ＞ 98% of cause property.The particle size of gained metatitanic acid is 1.2-1.5 μm, and the reducing power of product is preferable.
Preheating can shorten the heating-up time, promote titanium hydrolysis quickly to carry out, although under study for action it was found that pre-
Heat has above-mentioned advantage, but easily causes that initial stage hydrolysis rate is too fast, and hydrolysate particle size differs, to solve the problem,
We have passed through a series of exploration and analysis, by selecting total titanium concentration TiO2215-235g/L、Ti3+Concentration 1.0-3.0g/
L, sour ratio 1.7-2.0, Fe2+/TiO20.27-0.31, stability >=500ml, solid formation≤30mg/L titanium sulfate liquid, control
The volume ratio of desalted water processed and titanium sulfate liquid is 20-25%, by the technique of the micro-boiling twice of step B, D, curing, is successfully solved
The problem of initial stage, hydrolysis rate was too fast, and hydrolysate particle size differs, while ensure that hydrolysis rate at initial stage, shorten water
Solve the time.Unexpectedly, when addition boiling desalted water is diluted hydrolysis on the basis of the above, the hydrolysis effect in hydrolysis later stage is improved
Rate, detection find the phase after hydrolyzing, and low concentration titanium hydrolysis carries out fully, improving metatitanic acid particle growth.Above-mentioned operation and
The strict control of parameter, raw material, make the hydrolysate metatitanic acid particle of acquisition uniform in size on the whole, percent hydrolysis ＞ 98%.
Titanium sulfate liquid addition the time control and the heating-up time control, avoid high concentration overheat titanium liquid itself into
Core, the problem of new hydrolysis metatitanic acid small particles is produced, further ensuring hydrolysate metatitanic acid particle, size is equal on the whole
Even property.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
(1) titanium sulfate solution preheats：Titanium sulfate liquid 1000ml is taken in 2000ml beakers, resistance stove heat, control heating
1 DEG C/min of speed, is heated to 98 DEG C.Titanium sulfate liquid quality index：1. total titanium concentration TiO2225.21g/L；②Ti3+Concentration
1.89g/L；3. sour ratio 1.81；④Fe2+/TiO20.29；5. stability 530ml, stability are also known as stability, in titanium dioxide
In production, titanium liquid has generation early stage hydrolysis and to separate out white metatitanic acid (or positive metatitanic acid) colloid micro- in the case where condition changes
The tendency of grain, the degree of strength of this tendency are called the stability of titanium liquid, represent that the strong and weak characteristic of this tendency is called stability,
Ml number table of the stability of titanium liquid with every ml titaniums liquid with 25 DEG C of distilled water dilutings to required distilled water when just there is white opacity
Show；6. solid formation 12.3mg/L, solid formation is colloidal particles caused by residue and early stage hydrolysis.
(2) desalted water is preheating to 100.5 DEG C of boiling.
Plus bottom water (3)：The desalted water 250ml to have seethed with excitement is added in the 2000ml beakers with stirring, is turned by 40-80r/min
Speed is stirred.
Plus titanium sulfate liquid (4)：Preheated titanium sulfate liquid is added in the beaker of step (3), adds 16 minutes time.
(5) heating boiling：After titanium sulfate liquid adds, stir 5 minutes, be stirred, be warming up to micro- by 40-80r/min rotating speeds
Boiling, 115 DEG C of temperature, the heating-up time, temperature control hydrolyzed 37 minutes at 115-118 DEG C at 18 minutes, and hot water is added dropwise and keeps liquid
Position, slurry become steel helmet color.
(6) cure：When hydrolysis slurry becomes steel helmet color (percent hydrolysis is 58.23%), stopping stirring, heating.30 points of curing
Clock.
(7) secondary boiling：Open stirring and be warming up to micro-boiling, be stirred by 40-80r/min rotating speeds, 116 DEG C of temperature, control
Heating-up time at 18 minutes, controls 116-118 DEG C of temperature, and hot water is added dropwise and keeps liquid level, hydrolyzes 180min.
(8) dilute：Boiling desalted water is rapidly joined, controls total titanium concentration TiO in slurry2162.54g/L keep slurry micro-
Boiling, 108-112 DEG C of temperature, hydrolyze 60min.
(9) hydrolysis terminates.
Embodiment 2
(1) titanium sulfate solution preheats：Titanium sulfate liquid 1000ml is taken in 2000ml beakers, resistance stove heat, control heating
1 DEG C/min of speed, is heated to 96 DEG C.Titanium sulfate liquid quality index：1. total titanium concentration TiO2231.45g/L；②Ti3+Concentration
2.45g/L；3. sour ratio 1.76；④Fe2+/TiO20.27；5. stability 500ml；6. solid formation 10.4mg/L.
(2) desalted water is preheating to 99 DEG C of boiling.
Plus bottom water (3)：The desalted water 250ml to have seethed with excitement, stirring are added in the 2000ml beakers with stirring.
Plus titanium sulfate liquid (4)：Preheated titanium sulfate liquid is added in the beaker of step (3), adds 17 minutes time.
(5) heating boiling：After titanium sulfate liquid adds, stir 5 minutes, be warming up to micro-boiling, 114 DEG C of temperature, the heating-up time exists
17 minutes, temperature control hydrolyzed 41 minutes at 114-118 DEG C, and slurry becomes steel helmet color.
(6) cure：When hydrolysis slurry becomes steel helmet color (percent hydrolysis is 55.68%), stopping stirring, heating.30 points of curing
Clock.
(7) secondary boiling：Open stirring and be warming up to micro-boiling, 118 DEG C of temperature, the control heating-up time at 19 minutes, controls temperature
116-118 DEG C, hot water is added dropwise and keeps liquid level, hydrolyzes 180min.
(8) dilute：Boiling desalted water is rapidly joined, controls total titanium concentration TiO in slurry2164.54g/L keep slurry micro-
Boiling, 108-112 DEG C of temperature, hydrolyze 60min.
(9) hydrolysis terminates.
Embodiment 3
(1) titanium sulfate solution preheats：Titanium sulfate liquid 1000ml is taken in 2000ml beakers, resistance stove heat, control heating
1 DEG C/min of speed, is heated to 98 DEG C.Titanium sulfate liquid quality index：1. total titanium concentration TiO2233.18g/L；②Ti3+Concentration
2.57g/L；3. sour ratio 1.72；④Fe2+/TiO20.27；5. stability 515ml；6. solid formation 21.3mg/L.
(2) desalted water is preheating to 101 DEG C of boiling.
Plus bottom water (3)：The desalted water 250ml to have seethed with excitement, stirring are added in the 2000ml beakers with stirring.
Plus titanium sulfate liquid (4)：Preheated titanium sulfate liquid is added in the beaker of step (3), adds 18 minutes time.
(5) heating boiling：After titanium sulfate liquid adds, stir 5 minutes, be warming up to micro-boiling, 118 DEG C of temperature, the heating-up time exists
18 minutes, temperature control hydrolyzed 43 minutes at 112-118 DEG C, and slurry becomes steel helmet color.
(6) cure：When hydrolysis slurry becomes steel helmet color (percent hydrolysis is 62.02%), stopping stirring, heating.30 points of curing
Clock.
(7) secondary boiling：Open stirring and be warming up to micro-boiling, 116 DEG C of temperature, the heating-up time at 17 minutes, controls temperature 116-
118 DEG C, hot water is added dropwise and keeps liquid level, hydrolyzes 180min.
(8) dilute：Boiling desalted water is rapidly joined, controls total titanium concentration TiO in slurry2169.14g/L keep slurry micro-
Boiling, 108-112 DEG C of temperature, hydrolyze 60min.
(9) hydrolysis terminates.
The various embodiments described above sample makes the detection of melamine laminated paper by neat peak green wood decorating base paper experimental test procedures
Laminated paper covering power：Single-steeping, body paper full penetration (the melmac mixed liquor modulated) are dried afterwards；It will rise impermeable
Form mixed uniformly suspension in the melmac that the titanium dioxide slurry of bright effect is added after modulation, in secondary coating on
Quantitative mixed liquor is coated on lower two sides, and paper is uniformly fixed to after drying, is detected after overlaying.Reference selects domestic sulfuric acid
Method decorating base paper titanium dioxide primary product (without coating processing), laminated paper detection covering power is prepared with same method.Use Malvern
Laser particle analyzer tests the particle diameter of titanium dioxide.Test result see the table below 1.
Table 1, titanium dioxide particle diameter and impregnation laminated paper opacity
| Sample ID | Median particle diameter, μm | Span, μm | Laminated paper opacity |
| Example 1 | 0.490 | 0.932 | 91.23% |
| Example 2 | 0.489 | 0.927 | 91.45% |
| Example 3 | 0.492 | 0.930 | 91.38% |
| R—917 | 0.403 | 1.542 | 90.31% |
| R—952 | 0.619 | 1.517 | 90.19% |
As can be seen from the above table, the median particle diameter and particle diameter distribution span of embodiment sample are understood, present invention control titanium white powder
Footpath is preferable, and titanium dioxide melamine laminated paper covering power is higher 1 than domestic well-known sulfuric acid process famous brand name laminated paper opacity
More percentage points, titanium dioxide 10% or so can be saved.
Claims (7)
- A kind of 1. method for controlling decorating base paper titanium dioxide particle diameter, it is characterised in that by controlling hydrolyzing process, including following step Suddenly：A, from total titanium concentration TiO2215-235g/L、Ti3+Concentration 1.0-3.0g/L, sour ratio 1.7-2.0, Fe2+/TiO2 0.27-0.31, stability >=500ml, solid formation≤30mg/L titanium sulfate liquid, are preheating to 96-98 DEG C, standby；By desalted water Boiling is preheated to, it is standby；B, the desalted water for being preheated to boiling is charged first in hydrolysis reactor, stirred, then add the titanium sulfate liquid of preheating, control The volume ratio of desalted water processed and titanium sulfate liquid is 20-25%, after titanium sulfate liquid adds, stirring, is heated to micro-boiling；C, treat that step B percent hydrolysis reaches 50-65%, stop stirring, stop heating, cured；D, after curing, it is stirred again, is heated to micro-boiling 160-180min is hydrolyzed；E, boiling desalted water is added, controls total titanium concentration TiO in slurry2160-180g/L, micro-boiling is kept, hydrolyze 50-60min.
- 2. a kind of method for controlling decorating base paper titanium dioxide particle diameter according to claim 1, it is characterised in that in step B The temperature of micro-boiling is 112-118 DEG C, and it is 18-20min to control the heat temperature raising time.
- A kind of 3. method for controlling decorating base paper titanium dioxide particle diameter according to claim 1, it is characterised in that the temperature of curing Spend and be, the time of curing is 20-30min.
- 4. a kind of method for controlling decorating base paper titanium dioxide particle diameter according to claim 1, it is characterised in that in step D The temperature of micro-boiling is 114-118 DEG C, and it is 18-20min to control the heat temperature raising time.
- 5. a kind of method for controlling decorating base paper titanium dioxide particle diameter according to claim 1, it is characterised in that in step E The temperature of micro-boiling is 108-112 DEG C.
- 6. a kind of method for controlling decorating base paper titanium dioxide particle diameter according to claim 1, it is characterised in that in step A From total titanium concentration TiO2225-235g/L、Ti3+Concentration 1.0-3.0g/L, sour ratio 1.7-1.85, Fe2+/TiO2 0.27- 0.29th, stability >=500ml, solid formation≤30mg/L titanium sulfate liquid.
- A kind of 7. method for controlling decorating base paper titanium dioxide particle diameter according to claim 1, it is characterised in that in step E, Boiling desalted water is added, controls total titanium concentration TiO in slurry2160-170g/L。
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Cited By (1)
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