CN107500347B - A method of control decorating base paper titanium dioxide partial size - Google Patents

A method of control decorating base paper titanium dioxide partial size Download PDF

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CN107500347B
CN107500347B CN201710790698.5A CN201710790698A CN107500347B CN 107500347 B CN107500347 B CN 107500347B CN 201710790698 A CN201710790698 A CN 201710790698A CN 107500347 B CN107500347 B CN 107500347B
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boiling
titanium
base paper
titanium dioxide
decorating base
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CN107500347A (en
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张建平
张川
张千
张潇
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HEBEI MILSON TITANIUM DIOXIDE CO Ltd
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HEBEI MILSON TITANIUM DIOXIDE CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63Inorganic compounds
    • D21H17/67Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/675Oxides, hydroxides or carbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

A method of control decorating base paper titanium dioxide partial size belongs to the technical field of decorating base paper titanium dioxide, passes through control hydrolyzing process, comprising the following steps: and titanium sulfate liquid A, is selected, is preheating to 96-98 DEG C, it is spare;Desalted water is preheated to boiling, it is spare;B, the desalted water for being preheated to boiling is charged first in hydrolysis reactor, stirs, the titanium sulfate liquid of preheating is then added, after titanium sulfate liquid adds, stirring is heated to micro-boiling;C, 50-65% is reached to the percent hydrolysis of step B, stops stirring, stops heating, is cured;D, it after curing, 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 keeps micro-boiling, hydrolyzes 50-60min.The method of the present invention makes titanium sulfate liquid pyrohydrolysis technology meet decorating base paper requirement implementation, 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

A method of control decorating base paper titanium dioxide partial size
Technical field
The invention belongs to the technical fields of decorating base paper titanium dioxide, are related to the research of decorating base paper titanium dioxide partial size, specifically It is related to a kind of method for controlling decorating base paper titanium dioxide partial size.It is former that the method for the present invention makes titanium sulfate liquid pyrohydrolysis technology meet decoration 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 starting with from technology for hydrolyzing, the titanium dioxide partial size prepared with sulfuric acid process is set to reach the advantage of chloridising, and then make to prepare Decorating base paper either covering power, whiteness, gloss all compare favourably with Titanium Dioxide Produced by Chloride Procedure.
Background technique
Decorating base paper is one kind using the pigments and fillers such as high-quality wood pulp and titanium dioxide (accounting for 30% or so) as work made of Raw material processing Industry speciality 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:Whiteness height, good luster;Covering power is high;Good dispersion;It is weather-proof Property is good.One key factor of these characteristics of titanium dioxide is exactly the partial size of titanium dioxide, partial size of the decorating base paper to titanium dioxide It is required that being different from the fields such as coating, plastics.
There are two types of the titanium white production methods of decorating base paper, and one is sulfuric acid process, and one is chloridisings.Global sulfuric acid process produces Can about 50%, production capacity account for global half China based on sulfuric acid process, account for 95% or more production capacity.
Titanium sulfate liquid pyrohydrolysis is sulfuric acid method titanium pigment production center link, the main control target of pyrohydrolysis be exactly water and The partial size of titanium dioxide.The partial size of hydrated titanium dioxide determines the operating condition of subsequent handling and the optical property of product, 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 1970s, and new technical research there is no report Road.Chinese titanium dioxide industry was risen in the beginning of the nineties in last century, and this century is rapidly developed, but technical research is seldom, mainly Still the pervious technology of East European countries' 1970s is continued to use, some enterprises pass through some the zero of exchange study world sulfuric acid process The advanced experience of star, industry homogeneity is very serious, payes attention to the control of titanium dioxide partial size not enough, causing later period application effect It is good not as good as Titanium Dioxide Produced by Chloride Procedure effect.
Summary 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, and a kind of control method for meeting decorating base paper titanium dioxide partial size particular/special requirement is provided.By excellent Different technology for hydrolyzing achievees the effect that control decorating base paper titanium dioxide partial size, carrys out table with decorating base paper impregnation laminated paper opacity Levy the superiority and inferiority of titanium dioxide partial size.
The present invention be realize its purpose the technical solution adopted is that:
A method of control decorating base paper titanium dioxide partial size, by controlling hydrolyzing process, comprising the following steps:
A, total titanium concentration TiO is selected2215-235g/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, spare;It will take off Brine preheating is spare to boiling;
B, the desalted water for being preheated to boiling is charged first in hydrolysis reactor, stirs, the titanium sulfate of preheating is then added The volume ratio of liquid, control desalted water and titanium sulfate liquid is 20-25%, and after titanium sulfate liquid adds, stirring is heated to micro-boiling;
C, 50-65% is reached to the percent hydrolysis of step B, stops stirring, stops heating, is cured;
D, it after curing, 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 keeps micro-boiling, hydrolyzes 50- 60min。
The temperature of micro-boiling is 112-118 DEG C in step B, and the control heat temperature raising time is 18-20min.
The temperature of micro-boiling is 114-118 DEG C in step D, and the control heat temperature raising time is 18-20min.
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+/TiO2 0.27-0.29, 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 present invention are:
The hydrolysate metatitanic acid particle that the control of method for hydrolysis of the present invention makes 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, and titanium hydrolysis is promoted quickly to carry out, although under study for action it was found that pre- Heat has above-mentioned advantage, but easily causes initial stage hydrolysis rate too fast, and hydrolysate particle size is different, to solve this 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+/TiO2 0.27-0.31, stability >=500ml, solid formation≤30mg/L titanium sulfate liquid, control The volume ratio of desalted water processed and titanium sulfate liquid is that 20-25% is successfully solved by the technique of step B, D micro-boiling twice, curing Initial stage hydrolysis rate is too fast, hydrolysate particle size different problem, while ensure that initial stage hydrolysis rate, shortens 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 period is improved Rate, phase, low concentration titanium hydrolysis carry out sufficiently, improving metatitanic acid particle growth after hydrolyzing for detection discovery.Above-mentioned operation and Parameter, the strict control of raw material keep the hydrolysate metatitanic acid particle obtained 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 at Core leads to the problem of new hydrolysis metatitanic acid small particles, and further ensuring hydrolysate metatitanic acid particle, size is equal on the whole Even property.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
Embodiment 1
Titanium sulfate solution preheating: taking titanium sulfate liquid 1000ml in 2000ml beaker, resistance stove heating, control heating speed 1 DEG C/min is spent, is heated to 98 DEG C.Titanium sulfate liquid quality index: total titanium concentration TiO2225.21g/L;Ti3+Concentration 1.89g/L;Acid Ratio 1.81;Fe2+/TiO20.29;Stability 530ml, stability are also known as stability, and in titanium white production, titanium liquid is in condition In the case where variation, have the tendency that early stage hydrolysis occurs and white metatitanic acid (or positive metatitanic acid) colloidal particles are precipitated, this tendency Degree of strength be called the stability of titanium liquid, indicate that the strong and weak characteristic of this tendency is called stability, the stability of titanium liquid is with every The ml number that ml titanium liquid is diluted to required distilled water when just there is white opacity with 25 DEG C of distilled water indicates;Solid formation 12.3mg/ L, solid formation are residue and the colloidal particles that early stage hydrolysis generates.
Desalted water is preheating to 100.5 DEG C of boiling.
Add bottom water: the desalted water 250ml to have boiled is added in the 2000ml beaker with stirring, by 40-80r/min revolving speed It is stirred.
Add titanium sulfate liquid: preheated titanium sulfate liquid being added in the beaker of step, is added the time 16 minutes.
Heating boiling: it after titanium sulfate liquid adds, stirs 5 minutes, is stirred, is warming up to slightly boiled by 40-80r/min revolving speed It rises, 115 DEG C of temperature, the heating-up time, temperature was controlled at 115-118 DEG C, is hydrolyzed 37 minutes at 18 minutes, and hot water is added dropwise and keeps liquid Position, slurry become steel helmet color.
Curing: when hydrolysis slurry becomes steel helmet color (percent hydrolysis is 58.23%), stopping stirring being heated.Curing 30 minutes.
Secondary boiling: opening stirring and be warming up to micro-boiling, is stirred by 40-80r/min revolving speed, and 116 DEG C of temperature, control rises The warm time at 18 minutes, controls 116-118 DEG C of temperature, and hot water is added dropwise and keeps liquid level, hydrolyzes 180min.
Dilution: rapidly joining boiling desalted water, controls total titanium concentration TiO in slurry2162.54g/L keeping slurry slightly boiled It rises, 108-112 DEG C of temperature, hydrolyzes 60min.
Hydrolysis terminates.
Embodiment 2
Titanium sulfate solution preheating: taking titanium sulfate liquid 1000ml in 2000ml beaker, resistance stove heating, control heating speed 1 DEG C/min is spent, is heated to 96 DEG C.Titanium sulfate liquid quality index: total titanium concentration TiO2231.45g/L;Ti3+Concentration 2.45g/L;Acid Ratio 1.76;Fe2+/TiO20.27;Stability 500ml;Solid formation 10.4mg/L.
Desalted water is preheating to 99 DEG C of boiling.
Add bottom water: the desalted water 250ml to have boiled is added in the 2000ml beaker with stirring, stirs.
Add titanium sulfate liquid: preheated titanium sulfate liquid being added in the beaker of step, is added the time 17 minutes.
Heating boiling: it after titanium sulfate liquid adds, stirs 5 minutes, is warming up to micro-boiling, 114 DEG C of temperature, the heating-up time is 17 Minute, temperature is controlled at 114-118 DEG C, is hydrolyzed 41 minutes, and slurry becomes steel helmet color.
Curing: when hydrolysis slurry becomes steel helmet color (percent hydrolysis is 55.68%), stopping stirring being heated.Curing 30 minutes.
Secondary boiling: it opens stirring and is warming up to micro-boiling, 118 DEG C of temperature, control the heating-up time at 19 minutes, control temperature 116-118 DEG C, hot water is added dropwise and keeps liquid level, hydrolyzes 180min.
Dilution: rapidly joining boiling desalted water, controls total titanium concentration TiO in slurry2164.54g/L keeping slurry slightly boiled It rises, 108-112 DEG C of temperature, hydrolyzes 60min.
Hydrolysis terminates.
Embodiment 3
Titanium sulfate solution preheating: taking titanium sulfate liquid 1000ml in 2000ml beaker, resistance stove heating, control heating 1 DEG C/min of speed, is heated to 98 DEG C.Titanium sulfate liquid quality index:Total titanium concentration TiO2233.18g/L;Ti3+Concentration 2.57g/L;Sour ratio 1.72;Fe2+/TiO20.27;Stability 515ml;Solid formation 21.3mg/L.
Desalted water is preheating to 101 DEG C of boiling.
Add bottom water: the desalted water 250ml to have boiled is added in the 2000ml beaker with stirring, stirs.
Add titanium sulfate liquid: step is added in preheated titanium sulfate liquidBeaker in, be added the time 18 minutes.
Heating boiling: it after titanium sulfate liquid adds, stirs 5 minutes, is warming up to micro-boiling, 118 DEG C of temperature, the heating-up time exists 18 minutes, temperature was controlled at 112-118 DEG C, is hydrolyzed 43 minutes, and slurry becomes steel helmet color.
Curing: when hydrolysis slurry becomes steel helmet color (percent hydrolysis is 62.02%), stopping stirring being heated.30 points of curing Clock.
Secondary boiling: it opens stirring and is 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.
Dilution: rapidly joining boiling desalted water, controls total titanium concentration TiO in slurry2169.14g/L keeping slurry micro- Boiling, hydrolyzes 60min by 108-112 DEG C of temperature.
Hydrolysis terminates.
The various embodiments described above sample is by the production melamine laminated paper detection of neat peak green wood decorating base paper experimental test procedures Laminated paper covering power: single-steeping, body paper full penetration (the melamine resin mixed liquor modulated) are dried afterwards;It will rise impermeable The titanium dioxide slurry of bright effect is added in modulated melamine resin and forms mixed uniformly suspension, 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) prepares laminated paper detection covering power with same method.Use Malvern The partial size of laser particle analyzer test titanium dioxide.Test result see the table below 1.
As can be seen from the above table, the median particle diameter and particle diameter distribution span of embodiment sample are it is found that the present invention controls titanium white powder Diameter is preferable, and titanium dioxide melamine laminated paper covering power is 1 higher than domestic well-known sulfuric acid process famous brand name laminated paper opacity More percentage points can save titanium dioxide 10% or so.

Claims (6)

1. a kind of method for controlling decorating base paper titanium dioxide partial size, which is characterized in that by controlling hydrolyzing process, including following step It is rapid:
A, total titanium concentration TiO is selected2215-235g/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, spare;By desalted water It is preheated to boiling, it is spare;
B, the desalted water for being preheated to boiling is charged first in hydrolysis reactor, stirs, the titanium sulfate liquid of preheating is then added, controlled The volume ratio of desalted water processed and titanium sulfate liquid is 20-25%, and after titanium sulfate liquid adds, stirring is heated to micro-boiling;
C, 50-65% is reached to the percent hydrolysis of step B, stops stirring, stops heating, is cured;
D, it after curing, 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 keeps micro-boiling, hydrolyzes 50-60min.
2. a kind of method for controlling decorating base paper titanium dioxide partial size according to claim 1, which is characterized in that in step B The temperature of micro-boiling is 112-118 DEG C, and the control heat temperature raising time is 18-20min.
3. a kind of method for controlling decorating base paper titanium dioxide partial size according to claim 1, which is characterized in that in step D The temperature of micro-boiling is 114-118 DEG C, and the control heat temperature raising time is 18-20min.
4. a kind of method for controlling decorating base paper titanium dioxide partial size according to claim 1, which is characterized in that in step E The temperature of micro-boiling is 108-112 DEG C.
5. a kind of method for controlling decorating base paper titanium dioxide partial size according to claim 1, which is characterized in that in step A Select total titanium concentration TiO2225-235g/L、Ti3+Concentration 1.0-3.0g/L, sour ratio 1.7-1.85, Fe2+/TiO2 0.27- 0.29, stability >=500ml, solid formation≤30mg/L titanium sulfate liquid.
6. a kind of method for controlling decorating base paper titanium dioxide partial size according to claim 1, which is characterized in that in step E, Boiling desalted water is added, controls total titanium concentration TiO in slurry2160-170g/L。
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CN101607737B (en) * 2009-07-30 2011-06-29 攀钢集团攀枝花钢铁研究院有限公司 Method for producing titanium dioxide
CN101913647B (en) * 2010-08-31 2013-01-16 攀钢集团钢铁钒钛股份有限公司 Hydrolysis method for producing electronic-grade special titanium white by sulfuric acid process
CN102303904B (en) * 2011-08-11 2013-06-05 四川龙蟒钛业股份有限公司 Hydrolysis method for preparing high-brightness rutile titanium white from low-concentration titaniferous solution
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