CN105044282B - Degree detection device and method is hydrolyzed in early days in a kind of black titanium liquid acid hemolysis process of titanium white - Google Patents
Degree detection device and method is hydrolyzed in early days in a kind of black titanium liquid acid hemolysis process of titanium white Download PDFInfo
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- CN105044282B CN105044282B CN201510380301.6A CN201510380301A CN105044282B CN 105044282 B CN105044282 B CN 105044282B CN 201510380301 A CN201510380301 A CN 201510380301A CN 105044282 B CN105044282 B CN 105044282B
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Abstract
The present invention proposes the detection means of early stage hydrolysis degree and detection method in a kind of titanium white black titanium liquid acid hemolysis process, and described detection means includes：Blow-off valve, buchner funnel, bottle,suction, safety flack, ball valve, VRV, vacuum pump and connecting line, the vacuum orifice of vacuum pump is connected to safety flack by connecting line, and ball valve and VRV are provided with connecting line, safety flack is connected to bottle,suction by connecting line, buchner funnel is installed on the bottleneck of bottle,suction, and blow-off valve is arranged in the drainage line of bottle,suction.Described detection method includes：Close blow-off valve and ball valve, qualitative filter paper is laid in buchner funnel bottom, add water moistening, black titanium liquid to be measured is poured in buchner funnel, opens ball valve and carry out vacuum filtration timing, finally by timing result and the relative analyses of standard comparison time, obtain hydrolysis degree.The present invention initiates ground and quantifies to detect black titanium early stage hydrolysis degree with sucking filtration speed, and early stage hydrolysis detection limit has a extensive future.
Description
Technical field
The present invention relates to chemical industry measurement technical field, more particularly relate to a kind of morning in acid hemolysis process for titanium white black titanium liquid
The detection means of phase hydrolysis degree and method.
Background technology
Acidolysis is first chemical reaction process during sulfate process titanium dioxide produces, and its effect is by ilmenite concentrate with sulphuric acid
Titanium elements extract, and change into the titanyl sulfate solution of black（Hereinafter referred to as black titanium liquid）, after supply, operation produces, and final production goes out white
Titania powder（Titanium dioxide）.In the hydrolysis procedure of Producing Titanium Dioxide, affected by raw material or operating condition, black titanium liquid meeting
Produce different degrees of early stage hydrolysis, form colloid in black titanium liquid, reduce black titanium liquid in subsequent filter purification process
Deimpurity ability, and easily form irregular nucleus in follow-up hydrolyzing process, make particle diameter that hydrolysis produces from
Scattered property expands, and greatly reduces the pigment performance of end product.The early stage hydrolysis degree being directed to black titanium liquid in prior art only has
To judge from the reduction degree of the stability indicator of reducing solution, if reducing solution stability indicator reduction degree is larger, judging should
Batch black titanium liquid there occurs that in acid hemolysis process significant early stage hydrolyzes, this reduction degree based on reducing solution stability indicator
Traditional method to judge hydrolysis degree generally has that result of determination is inaccurate, it is larger to be affected by operating environment and operating time
Etc. defect, can only be used for determining whether roughly to occur the hydrolysis of highly significant, cannot judge for slight hydrolysis degree.Existing
A kind of effective ways detecting hydrolysis degree in black titanium liquid acid hemolysis process that can be relatively accurate not yet occur in technology.
Content of the invention
The present invention is based on above-mentioned prior art problem, and in conjunction with long-term production practices, the proposition of innovation is a kind of brand-new black
The detection means of hydrolysis degree and method in titanium liquid acid hemolysis process, the present invention has initiated black titanium hydrolysis degree detecting technology, its
Innovation is：Quantitative black titanium liquid is carried out sucking filtration under conditions of constant vacuum, measures its sucking filtration speed, and will survey
Amount result is compared with standard specimen numerical value, accurately judges early stage hydrolysis degree by this standard comparison, achieving first can
The black titanium hydrolysis degree detecting quantifying, substantially increases black titanium hydrolysis degree detecting precision, and operating process is simply easy
OK, with low cost, there is wide promotion prospect.
The technical scheme that present invention solution above-mentioned technical problem is taken is as follows：
The detection means of early stage hydrolysis degree in a kind of black titanium liquid acid hemolysis process of titanium white, including：Blow-off valve 1, buchner funnel
2nd, bottle,suction 3, safety flack 4, ball valve 5, VRV 6, vacuum pump 7 and connecting line, the vacuum orifice of described vacuum pump 7 leads to
Cross connecting line and be connected to safety flack 4, and ball valve 5 and VRV 6, described safety flack are provided with described connecting line
4 are connected to described bottle,suction 3 by connecting line, and described buchner funnel 2 is installed on the bottleneck of described bottle,suction 3, described discharge
Valve 1 is arranged in the drainage line of described bottle,suction 3.
Further according to detection means of the present invention, wherein said ball valve 5 is arranged at VRV 6 and safety
On connecting line between bottle 4, the bottleneck of described safety flack is sealed by the bottle stopper with dual circuit.
It is further that according to detection means of the present invention, wherein said bottle,suction 3 is upper and lower mouth taper bottle,suction,
Offer aspirating hole on the taper upper side wall of bottle,suction 3, described safety flack is connected to described aspirating hole by connecting line, taking out
The conical lower portion of filter flask 3 offers relief hole, and described relief hole is connected with marker pipe, and described marker pipe is installed
State blow-off valve 1, the open top of described bottle,suction is sealedly connected with described buchner funnel 2 by bottle stopper.
It is further that according to detection means of the present invention, wherein said buchner funnel is the buchner funnel of φ 80mm,
Described bottle,suction is the taper bottle,suction of mouth up and down of 1000ml, can make described safety by described vacuum pump 7 and VRV 6
Vacuum in bottle 4 and bottle,suction 3 is maintained at below -0.04Mpa.
The inspection of early stage hydrolysis degree in a kind of titanium white black titanium liquid acid hemolysis process being carried out based on detection means of the present invention
Survey method, comprises the following steps：
Step one, making standard specimen black titanium liquid, obtain the standard comparison time, specifically include：
1）, take the black titanium liquid of scheduled volume on production line, add sufficient active carbon dust fully to adsorb hydrocolloid therein；
2）, black titanium liquid is carried out a sucking filtration by above-mentioned detection device, remove the colloid of absorption and unnecessary activated carbon
Powder；
3）, to the appropriate necessary impurity of the above-mentioned supplement of the black titanium liquid through a sucking filtration, the black titanium liquid of prepared standard specimen, and so that
Standard specimen black titanium liquid and black titanium liquid phase to be measured are only that in the black titanium liquid of standard specimen than difference and eliminate hydrocolloid；
4）, by after black for above-mentioned standard specimen titanium liquid extraction standard amount, sucking filtration timing is carried out by above-mentioned detection device, obtains standard
Comparison time, concrete sucking filtration timing course is：
4.1st, close blow-off valve 1 and ball valve 5, start vacuum pump 7 and carry out evacuation；
4.2nd, qualitative filter paper is laid in the bottom of buchner funnel, adds appropriate water-wet and make filter paper be close to buchner funnel
Bottom, opens ball valve, and in funnel, water closes ball valve when being filtered dry；
4.3rd, after black for the standard specimen of above-mentioned standard amount titanium liquid being heated to predetermined temperature and stirs, pour buchner funnel 4 into
Interior, open ball valve 5 and carry out vacuum filtration, start simultaneously at timing, until stopping timing after standard specimen black titanium liquid is filtered dry in buchner funnel,
Close ball valve 5, the sucking filtration time being recorded is i.e. as the standard comparison time.
Step 2, according to above-mentioned standard amount extract isodose to be measured black titanium liquid, sucking filtration is carried out by above-mentioned detection device
Timing, obtains the sucking filtration time of black titanium liquid to be measured, and concrete sucking filtration timing course includes：
1）, close blow-off valve 1 and ball valve 5, start vacuum pump 7 and carry out evacuation；
2）, qualitative filter paper is laid in the bottom of buchner funnel, add appropriate water-wet simultaneously to make filter paper be close to buchner funnel
Bottom, opens ball valve, and in funnel, water closes ball valve when being filtered dry；
3）, the to be measured black titanium liquid of above-mentioned standard amount is heated to predetermined temperature and stirs after, pour buchner funnel 4 into
Interior, open ball valve 5 and carry out vacuum filtration, start simultaneously at timing, until stopping timing after black titanium liquid to be measured is filtered dry in buchner funnel,
Close ball valve 5, the sucking filtration time being recorded is the sucking filtration time of black titanium liquid to be measured.
The standard of the standard specimen black titanium liquid that step 3, the to be measured black titanium liquid sucking filtration time that step 2 is surveyed and step one determine
Comparison time is compared, so that it is determined that the early stage hydrolysis degree of black titanium liquid to be measured.
Further according to detection method of the present invention, wherein the 2nd of step one）A sucking filtration process in small step
Including：
1）, close blow-off valve 1 and ball valve 5, start vacuum pump 7 and carry out evacuation；
2）, qualitative filter paper is laid in the bottom of buchner funnel, add appropriate water-wet simultaneously to make filter paper be close to buchner funnel
Bottom, opens ball valve, and in funnel, water closes ball valve when being filtered dry, and closes discharge after opening the water that blow-off valve is discharged in bottle,suction
Valve；
3）, black titanium liquid is heated to predetermined temperature and stirs after, pour in buchner funnel 4, open ball valve 5 and carry out very
Empty sucking filtration, in funnel, black titanium liquid closes ball valve 5 when being filtered dry, and opens blow-off valve 1, extracts the black titanium liquid through a sucking filtration.
Further according to detection method of the present invention, wherein the 3rd in step one）In small step, to through once taking out
The filter mud that the black titanium liquid supplement of filter is appropriate is obtained standard specimen black titanium liquid, and the addition of described filter mud is according to filter mud in black titanium liquid to be measured
It is determined containing concentration it is ensured that standard specimen black titanium liquid contains equal impurity with black titanium liquid phase to be measured in vitro than eliminating water dispergation.
Further according to detection method of the present invention, wherein the 3rd of step 2）In small step, black titanium liquid to be measured adds
Hot temperature and sucking filtration vacuum and the heating-up temperature of standard specimen black titanium liquid and sucking filtration vacuum corresponding one in the 4th small step of step one
Cause.
Further according to detection method of the present invention, black titanium liquid to be measured and standard specimen in step one wherein in step 2
Black titanium liquid is extracted from same production line source.
The inspection of early stage hydrolysis degree in a kind of titanium white black titanium liquid acid hemolysis process being carried out based on detection means of the present invention
Survey method, comprises the following steps：
Step one, making standard specimen black titanium liquid, obtain the standard comparison time, specifically include：
1）, take the black titanium liquid of 200ml on production line, add the activated carbon powder of 0.1g 325 mesh fully to adsorb hydrolysis glue therein
Body；
2）, close blow-off valve 1 and ball valve 5, start vacuum pump 7, adjustment VRV 6 is so that vacuum is -0.04
～-0.05Mpa；
3）, two φ 70mm qualitative filter papers are entirely placed in buchner funnel 2 bottom of φ 80mm, add 20ml water, open
Open ball valve 5, close ball valve 5 when water is filtered dry, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom, the then row of opening
Blow-off valve 1 is closed after water in material valve 1 discharge bottle,suction；
4）, by the black titanium liquid of above-mentioned 200ml, be heated to 68～70 DEG C, stir, pour buchner funnel 4 into, open ball valve
5 carry out sucking filtration, after titanium liquid sample black in funnel is drained, close ball valve 5, open blow-off valve extraction black after a sucking filtration
Titanium liquid；
5）, add 0.5g filter mud in the black titanium of the 200ml once liquid to above-mentioned sucking filtration, after stirring, extract the black titanium of 50ml
Liquid is as standard specimen black titanium liquid, and is heated to 68～70 DEG C；
6）, close blow-off valve 1 and ball valve 5, start vacuum pump 7, adjustment VRV 6 is so that vacuum is -0.04
～-0.05Mpa；
7）, the qualitative filter paper of two φ 70mm is entirely placed in buchner funnel 2 bottom of φ 80mm, add 20ml water,
Open ball valve 5, close ball valve 5 when water is filtered dry, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom；
8）, black for above-mentioned 50ml standard specimen titanium liquid is heated to 68～70 DEG C, stir, pour buchner funnel 4 again into, open
Ball valve 5, adjustment VRV 6, it is ensured that vacuum is in -0.04～-0.05Mpa, starts sucking filtration, and starts timing；
9）, the black titanium liquid of the standard specimen in buchner funnel 2 is when being filtered dry, stop timing, close ball valve 5, during the sucking filtration being recorded
Between as standard comparison time t0.
Step 2, extraction black titanium liquid to be measured, detect the sucking filtration time, specifically include：
1）, close blow-off valve 1 and ball valve 5, start vacuum pump 7, adjustment VRV 6 is it is ensured that vacuum is -0.04
～-0.05Mpa；
2）, two φ 70mm qualitative filter papers are entirely placed in buchner funnel 2 bottom of φ 80mm, add 20ml water, open
Open ball valve 5, water filter is closed ball valve 5 when draining, qualitative filter paper lubricated and tiles and be close to buchner funnel bottom；
3）, on same production line extract 50ml black titanium liquid to be measured, be heated to 68～70 DEG C, stir, pour Bu Shi into
In funnel 4, open ball valve 5, adjustment VRV 6, it is ensured that vacuum is in -0.04～-0.05Mpa, starts sucking filtration, and starts
Timing；
4）, the to be measured black titanium liquid in buchner funnel 2 is when being filtered dry, and stops timing, closes ball valve 5, the time used by record is
Sucking filtration time t1 for black titanium liquid to be measured.
The mark of the standard specimen black titanium liquid that step 3, the to be measured black titanium liquid sucking filtration time t1 that step 2 is recorded and step one are demarcated
Quasi- comparison time t0 is analyzed, the standard comparison time of the sucking filtration time t1 based on black titanium liquid to be measured and standard specimen black titanium liquid
Departure degree between t0 judges the early stage hydrolysis degree of black titanium liquid to be measured.
Following technique effect at least can be reached by technical scheme：
1）, the present invention initiates ground and detects with sucking filtration speed, quantifies the early stage hydrolysis degree of acidolysis black titanium liquid it is achieved that one
Kind brand-new black titanium hydrolysis degree detecting technology, can wide popularization and application in the hydrolysis detection in Producing Titanium Dioxide, before market
Scape is wide.
2）, the present invention based on sucking filtration velocity standard compare principle achieve black titanium liquid early stage hydrolysis degree quantization detection,
Reduce the decision method of degree with respect to tradition by reducing solution stability indicator, substantially increase the detection of black titanium hydrolysis degree
Precision is it is ensured that the quality of end product.
3）, detection method of the present invention realized based on simple a set of testing equipment, whole detection process operation
Simply, with low cost.
Brief description
Accompanying drawing 1 is the acidolysis process process of existing titanium white black titanium liquid；
The titanium white black titanium hydrolysis degree detection device that accompanying drawing 2 provides for the present invention.
The implication of each reference of in figure is as follows：
1- blow-off valve, 2- buchner funnel, 3- bottle,suction, 4- safety flack, 5- ball valve, 6- VRV, 7- vacuum pump.
Specific embodiment
Below in conjunction with accompanying drawing, technical scheme is described in detail, so that those skilled in the art can be more
Plus be clearly understood from the solution of the present invention, but therefore do not limit the scope of the invention.
Combine accompanying drawing 1 first the acidolysis process process of titanium white black titanium liquid is briefly described, so as to clearer
Understanding the technical problem to be solved.As shown in Figure 1, the acid hemolysis process of titanium white black titanium liquid includes following main step
Suddenly：
（1）, the concentrated sulphuric acid of ilmenite concentrate and 93-98% is sufficiently mixed uniformly by compressed air（Premixing）, add water or
23% dilute sulfuric acid, is mixed the Macrodilution heat producing, ore deposit acid blend is heated beyond using the water in spent acid with concentrated sulphuric acid
After 100 DEG C, there is violent heat release primary response, more than 180 DEG C in several minutes, primary response terminates within 3～5 minutes, temperature gradually under
Fall.
（2）, generate cellular solid formation be maintained at 90～100 DEG C of ripenings 2 ~ 3 hours.
（3）, add quantitative water by the speed setting, the titanyl sulfate dissolving leaching in solid formation forms black titanium liquid,
Leaching process is maintained at 68～73 DEG C.
（4）, after leaching terminates, add iron filings or iron powder, the ferric iron back in black titanium liquid become ferrous irons, reduction process
Temperature is maintained at 68～73 DEG C.
（5）, after reduction terminates, black titanium liquid is mixed in proportion with flocculant, particulate matter is naturally heavy through 2～4 hours
Fall, filter the supernatant send rear operation, the solidliquid mixture of bottom send again after Filter Press after operation.
In above-mentioned acid hemolysis process, after leaching, reduction, affected by raw material, operating condition, generating unit can be hydrolyzed early stage and divide
Ti(OH)4Positive metatitanic acid and Ti (OH)2Metatitanic acid, is combined with other impurity shapes, forms colloid flocculent deposit or colloid, serious fall
Low black titanium liquid goes deimpurity ability, the performance of impact end product in subsequent filter purification process.It is right that the present invention passes through
The flocculent deposit producing in this hydrolytic process or colloid carry out detecting the size to judge hydrolyzing occurrence degree.
Accompanying drawing 2 provides the structural representation of titanium white of the present invention black titanium hydrolysis degree detection device, as accompanying drawing 2 institute
Show, whole detection means includes：Blow-off valve 1, buchner funnel 2, bottle,suction 3, safety flack 4, ball valve 5, VRV 6, vacuum
Pump 7 and connecting line, the vacuum orifice of described vacuum pump 7 is connected to safety flack 4 by pipeline, and arranges on described pipeline
There are ball valve 5 and VRV 6, wherein ball valve 5 closer to the position of safety flack, described safety flack is connected to by pipeline to be taken out
Filter flask 3, by the bottle stopper sealing with dual circuit, described bottle,suction 3 is conical flask to the bottleneck of safety flack, in bottle,suction 3
Aspirating hole is offered, described safety flack is sealedly attached to described aspirating hole by pipeline, described bottle,suction 3 on taper upper side wall
Conical lower portion offers relief hole, and described relief hole is connected to marker pipe, and described marker pipe is provided with blow-off valve.Institute
The open top stating bottle,suction is sealedly connected with buchner funnel 2 by bottle stopper, and solution can be entered by the bell mouth of buchner funnel
In bottle,suction, it is high leakproofness between each bottle of described detection means and pipeline and connects, be closed in blow-off valve, Bu Shi leakage
The bell mouth of bucket after liquid seal, is started vacuum pump, opening ball valve can be in bottle,suction 3, safety flack 4 and relevant connection pipeline
The vacuum of below formation -0.04Mpa.Preferably described buchner funnel is the buchner funnel of φ 80mm, and described bottle,suction is
The taper bottle,suction of mouth up and down of 1000ml.
The concrete detection method that using above-mentioned detection device carry out black titanium liquid early stage hydrolysis degree is given below, including following
Step：
Step one, the black titanium liquid standard specimen of making（Standard comparison sample）, obtain the standard comparison time, specifically include：
1）, take the black titanium liquid of the scheduled volume on production line, add enough activated carbon powders, fully inhaled by activated carbon powder comprehensively
Attached as the precipitation/colloid in the black titanium liquid of standard sample so that this black titanium liquid as standard sample be equivalently employed without send out
Gave birth to early stage hydrolysis（The colloid that hydrolysis produces all is absorbed）, then black titanium liquid is heated to predetermined temperature, this pre- constant temperature
The selection of degree preferably should ensure that make the black titanium liquid of standard sample, produce in be measured black titanium liquid and actual measurement in black
The temperature of titanium liquid should be consistent, reduces, by maximum, the measurement error that temperature contrast is brought.
2）, black titanium liquid is heated to after predetermined temperature carrying out a sucking filtration, carbon dust is removed completely by a this sucking filtration
The colloid absorbing and unnecessary activated carbon powder, one time sucking filtration process includes：After closing blow-off valve 1 and ball valve 5, start vacuum pump
7, device is carried out evacuation, then qualitative filter paper is laid in the bottom of buchner funnel, add suitable quantity of water to carry out moistening filter paper
And make filter paper be close to the bottom of buchner funnel, it is then turned on ball valve, water closes ball valve 5 when being filtered dry in funnel, then beats
Blow-off valve is closed after opening the water that blow-off valve is discharged in bottle,suction.Then the above-mentioned black titanium liquid being heated to predetermined temperature is stirred
Afterwards, pour in buchner funnel 4, open ball valve 5 and carry out vacuum filtration, after titanium liquid standard sample black in funnel is drained, close ball
Valve 5, opens blow-off valve, and the standard sample black titanium liquid through a sucking filtration is discharged by blow-off valve 1.
3）, to adding the filter mud of scheduled volume in the above-mentioned black titanium liquid of a sucking filtration and stir.Because by step
The rapid 2 black titanium liquid obtaining not only eliminate colloid and unnecessary activated carbon powder, eliminate wherein intrinsic also by sucking filtration simultaneously
The impurity such as filter mud, for obtaining accurate standard comparison result it is required that black titanium liquid and black titanium liquid to be measured as standard comparison sample
Compare, only remove the colloid wherein producing because of hydrolysis, and other the black titanium liquid to be measured beyond should not removing colloid also contain
Impurity, an above-mentioned sucking filtration process not only eliminates colloid in the black titanium liquid of standard comparison sample and its absorption carbon dust, and
And filter mud impurity part may have been filtered simultaneously.Black titanium liquid to be measured is derived from the black titanium liquid after reducing in acidolysis, in this black titanium liquid
In the major impurity part that contains be exactly filter mud, therefore for accurately carrying out standard comparison, need above-mentioned through a sucking filtration
Add the filter mud of scheduled volume in black titanium liquid afterwards, the addition of concrete filter mud can according in black titanium liquid to be measured filter mud contain concentration
（Empirical value, according to the difference of titanium ore, filter mud butt accounts for 2～10% by titanium dioxide total amount in titanium liquid）Determine, according to treating
The amount surveying filter mud concentration and the above-mentioned black titanium liquid through a sucking filtration in black titanium liquid can obtain the filter mud amount of needs addition（If
The hydrolysis degree of the black titanium liquid determining without impurity such as filter muds detected, then can save this step, directly with once taking out
Black titanium liquid after filter carries out sucking filtration timing, as long as ensureing that standard specimen black titanium liquid phase remove only hydrocolloid for black titanium liquid to be measured and is
Can）.
4）, black titanium liquid that step 3 obtained take standard volume post-heating to predetermined temperature, this standard volume is namely subsequently to be measured
The extracted amount of black titanium liquid, then carries out repeating sucking filtration：After closing blow-off valve 1 and ball valve 5, start vacuum pump 7, device is taken out
Then qualitative filter paper is laid in the bottom of buchner funnel, addition suitable quantity of water carries out moistening filter paper and so that filter paper is close to by vacuum
In the bottom of buchner funnel, it is then turned on ball valve, water closes ball valve 5 when being filtered dry in funnel.Again by the black titanium of above-mentioned standard amount
After liquid stirs, pour in buchner funnel 4, open ball valve 5 and carry out vacuum filtration, start simultaneously at timing until black titanium liquid is filtered dry
Stop timing afterwards, close ball valve, the sucking filtration time being recorded is i.e. as the standard comparison time.By ball valve 5 and VRV 6
Be able to ensure that and be in same vacuum in bottle during sucking filtration, if change or maintenance vacuum pump after, because rate of air sucked in required may be sent out
The larger change of life is it is therefore desirable to redeterminate standard specimen.
Step 2, extract commensurability to be measured black titanium liquid according to above-mentioned standard amount, and record black titanium to be measured in the manner described above
The sucking filtration time of liquid.This step not only requires black titanium liquid to be measured as the volume of above-mentioned standard specimen black titanium liquid, and requires both
It is extracted from same production line source, the colloid uniquely differing only in standard specimen black titanium liquid is filtered out, then will be extracted
Black titanium liquid to be measured carries out following sucking filtration：
1）, close blow-off valve 1 and ball valve 5 after, start vacuum pump 7, device carried out evacuation, vacuum and above-mentioned standard
Sucking filtration vacuum during comparison time makes is consistent；
2）, qualitative filter paper is laid in the bottom of buchner funnel, add suitable quantity of water to carry out moistening filter paper and make filter paper tight
It is affixed on the bottom of buchner funnel, is then turned on ball valve, water closes ball valve 5 when being filtered dry in funnel；
3）, the to be measured black titanium liquid of above-mentioned standard amount is heated to after above-mentioned predetermined temperature（With above-mentioned standard comparison time system
In work, the heating-up temperature of corresponding step standard specimen black titanium liquid is identical）, stir, pour in buchner funnel 4, open ball valve 5 and carry out
Vacuum filtration, and ensure that vacuum is consistent with the sucking filtration vacuum of standard specimen black titanium liquid during above-mentioned standard comparison time record, simultaneously
Start timing until black titanium liquid is filtered dry stopping timing, close ball valve, the sucking filtration time being recorded is the sucking filtration of black titanium liquid to be measured
Time.
The mark of the standard specimen black titanium liquid that step 3, the sucking filtration time of to be measured black titanium liquid that step 2 is surveyed and step one determine
Quasi- comparison time is compared, so that it is determined that the early stage hydrolysis degree of black titanium liquid to be measured.Because the colloid that black titanium hydrolysis produce
Can serious impact sucking filtration time, the size of hydrolysis degree and the proportional relation of colloid concentration producing, and colloid concentration with
The sucking filtration time is proportional, therefore under equal conditions, the size of the reflection hydrolysis degree that the sucking filtration time can be linear, can lead to
Demarcate after in advance, the comparing result of actual measurement sucking filtration time and standard comparison time is converted directly into intuitively hydrolysis degree detection
As a result, thus early stage black titanium liquid can accurately be detected by this method of the present invention very much occurring in acid hemolysis process
The size of hydrolysis degree.
The specific embodiment of the present invention is given below：
Embodiment 1
Below in conjunction with the acidolysis process of the black titanium liquid of titanium white shown in accompanying drawing 1, specifically give water in acid hemolysis process for the black titanium liquid
Solution degree detecting method example, comprises the following steps：
（One）Standard makes：
Take the black titanium liquid 200ml on production line, add the activated carbon powder of 0.1g 325 mesh（Enough）, fully adsorb wherein
Colloid, be then heated to 68～70 DEG C, sucking filtration once, comprises the steps：
1）, close blow-off valve 1 and ball valve 5, start vacuum pump 7, adjust VRV 6, vacuum -0.04～-
0.05Mpa；
2）, by two φ 70mm qualitative filter papers, be entirely placed in buchner funnel 2 bottom of φ 80mm, add 20ml water, open
Open ball valve 5, close ball valve 5 when water is filtered dry, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom, the then row of opening
Blow-off valve 1 is closed after water in material valve 1 discharge bottle,suction；
3）, by the black titanium liquid of above-mentioned 200ml, be heated to 68～70 DEG C, stir, pour buchner funnel 4 into, open ball valve
5 carry out sucking filtration, after titanium liquid sample black in funnel is drained, close ball valve 5, open blow-off valve, by the black titanium through a sucking filtration
Liquid is discharged by blow-off valve 1.
State then up and in sucking filtration black titanium liquid once, add pressure filter on production line to process the filter mud 0.5g after black titanium liquid
（Wet basis）It is ensured that the filter mud content in also black titanium liquid is basic with the filter mud content in the to be measured black titanium liquid of extracting directly on production line
Identical, after stirring, take 50ml black titanium liquid as standard specimen black titanium liquid, be heated to 68～70 DEG C, repeat to take out as follows
Filter step：
1）, close blow-off valve 1 and close ball valve 5, start vacuum pump 7, adjust VRV 6, vacuum is -0.04
～-0.05Mpa, during vacuum filtration, as long as opening ball valve, by VRV 6, you can ensure bottle,suction, safety flack
And its vacuum in pipeline is in -0.04～-0.05Mpa.
2）, by two φ 70mm qualitative filter papers（New）, entirely it is placed in buchner funnel 2 bottom of φ 80mm, add
20ml water, open ball valve 5, water take out in when close ball valve 5, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom.
3）, black for above-mentioned 50ml standard specimen titanium liquid is heated to 68～70 DEG C, stir, pour buchner funnel 4 again into, open
Ball valve 5, adjustment VRV 6, it is ensured that vacuum is in -0.04～-0.05Mpa, starts sucking filtration, and starts timing.
4）, the black titanium liquid sample of the standard specimen in buchner funnel 2 is when being filtered dry, stop timing, close ball valve 5, record institute's used time
Between i.e. as standard comparison time t0.
（Two）Detecting step：
1）, confirm blow-off valve 1 close, close ball valve 5, start vacuum pump 7, adjust VRV 6, vacuum-
0.04～0.05Mpa.
2）, by two φ 70mm qualitative filter papers, be entirely placed in buchner funnel 2 bottom of above-mentioned φ 80mm, add 20ml
Water, open ball valve 5, water take out in when close ball valve 5, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom.
3）, take same production line（With standard specimen black titanium liquid）On to be measured black titanium liquid 50ml, be heated to 68～70 DEG C, stirring is all
Even, pour buchner funnel 4 into, open ball valve 5, adjustment VRV 6, it is ensured that vacuum is in -0.04～-0.05Mpa, starts to take out
Filter, and start timing.
4）, the sample in buchner funnel 2 is when draining, stop timing, close ball valve 5, the time used by record is as to be measured
The sucking filtration time t1 of black titanium liquid.
（Three）Result compares：
By step（Two）The to be measured black titanium liquid sucking filtration time t1 recording and step（One）The standard comparison time t0 demarcated enters
Row relative analyses, you can obtain the early stage hydrolysis degree of black titanium liquid to be measured.
In the above-mentioned detection process of the present invention, it is always maintained at being tightly connected between each pipeline and assay flask, by vacuum pump
Ensure that with VRV the vacuum in bottle,suction, safety flack and its pipeline in whole detection process keeps constant, right
In the sucking filtration time of black titanium liquid, what impact was larger is exactly colloid therein and filter mud, and the present invention is in standard specimen making by excessive
Activated carbon has fully absorbed the colloid in standard specimen, simultaneously for ensureing only to absorb colloid, filters according in black titanium liquid to be measured in standard specimen
The filter mud of mud concentration special addition reasonable amount is it is ensured that the accuracy of testing result.Additionally while temperature, vacuum are to sucking filtration
The impact of time is less, and the present invention still ensure that to greatest extent during standard specimen makes and sample is surveyed, corresponding each
The temperature of step, vacuum are consistent the degree of accuracy it is ensured that testing result.
To sum up, the present invention initiates the early stage hydrolysis degree that ground detected, quantified acidolysis black titanium liquid with sucking filtration speed, solves
In Producing Titanium Dioxide, the accurate detection problem of black titanium hydrolysis degree is it is achieved that the high-precision metrization of black titanium liquid early stage hydrolysis degree is examined
Survey, reduce the decision method of degree with respect to tradition by reducing solution stability indicator, substantially increase black titanium hydrolysis degree
Accuracy of detection is it is ensured that the quality of end product, and the testing equipment that whole detection method is relied on is simple to operate, low cost
Honest and clean, the popularization and application of described detection method are greatly facilitated.
The above is only and the preferred embodiment of the present invention is described, technical scheme is not limited to
This, any known deformation that those skilled in the art are made on the basis of the major technique design of the present invention broadly falls into the present invention
Claimed technology category, the specific protection domain of the present invention is defined by the record of claims.
Claims (9)
1. in a kind of black titanium liquid acid hemolysis process of titanium white early stage hydrolysis degree detection method, described detection method is based on the black titanium of titanium white
In liquid acid hemolysis process, the detection means of early stage hydrolysis degree is carried out, and described detection means includes：Blow-off valve（1）, buchner funnel
（2）, bottle,suction（3）, safety flack（4）, ball valve（5）, VRV（6）, vacuum pump（7）And connecting line, described vacuum pump
（7）Vacuum orifice safety flack is connected to by connecting line（4）, and it is provided with ball valve on described connecting line（5）With true
Empty air relief valve（6）, described safety flack（4）Described bottle,suction is connected to by connecting line（3）, described buchner funnel（2）Install
In described bottle,suction（3）Bottleneck, described blow-off valve（1）It is arranged at described bottle,suction（3）Drainage line on, its feature exists
In described detection method comprises the following steps：
Step one, making standard specimen black titanium liquid, obtain the standard comparison time, specifically include：
（1）, take the black titanium liquid of scheduled volume on production line, add sufficient active carbon dust fully to adsorb hydrocolloid therein；
（2）, black titanium liquid is carried out a sucking filtration by described detection means, remove the colloid of absorption and unnecessary activated carbon powder；
（3）, to the appropriate necessary impurity of the above-mentioned supplement of the black titanium liquid through a sucking filtration, the black titanium liquid of prepared standard specimen, and make to mark
Sample black titanium liquid and black titanium liquid phase to be measured are only that in the black titanium liquid of standard specimen than difference and eliminate hydrocolloid；
（4）, by after black for above-mentioned standard specimen titanium liquid extraction standard amount, sucking filtration timing is carried out by described detection means, obtains standard ratio
To the time, concrete sucking filtration timing course is：
4.1st, close blow-off valve（1）And ball valve（5）, start vacuum pump（7）Carry out evacuation；
4.2nd, qualitative filter paper is laid in the bottom of buchner funnel, adds appropriate water-wet and make filter paper be close to buchner funnel bottom
Portion, opens ball valve, and in funnel, water closes ball valve when being filtered dry；
4.3rd, after black for the standard specimen of above-mentioned standard amount titanium liquid being heated to predetermined temperature and stirs, pour buchner funnel into（2）It is interior,
Open ball valve（5）Carry out vacuum filtration, start simultaneously at timing, until stopping timing after standard specimen black titanium liquid is filtered dry in buchner funnel,
Close ball valve（5）, the sucking filtration time being recorded is i.e. as the standard comparison time；
Step 2, according to above-mentioned standard amount extract isodose to be measured black titanium liquid, sucking filtration timing is carried out by described detection means,
Obtain the sucking filtration time of black titanium liquid to be measured, concrete sucking filtration timing course includes：
（1）, close blow-off valve（1）And ball valve（5）, start vacuum pump（7）Carry out evacuation；
（2）, qualitative filter paper is laid in the bottom of buchner funnel, add appropriate water-wet simultaneously to make filter paper be close to buchner funnel bottom
Portion, opens ball valve, and in funnel, water closes ball valve when being filtered dry；
（3）, the to be measured black titanium liquid of above-mentioned standard amount is heated to predetermined temperature and stirs after, pour buchner funnel into（2）It is interior,
Open ball valve（5）Carry out vacuum filtration, start simultaneously at timing, until stopping timing after black titanium liquid to be measured is filtered dry in buchner funnel,
Close ball valve（5）, the sucking filtration time of the sucking filtration time as black titanium liquid to be measured being recorded；
The standard comparison of the standard specimen black titanium liquid that step 3, the to be measured black titanium liquid sucking filtration time that step 2 is surveyed and step one determine
Time compares, so that it is determined that the early stage hydrolysis degree of black titanium liquid to be measured.
2. detection method according to claim 1 it is characterised in that wherein step one（2）Once taking out in small step
Filtration journey includes：
（1）, close blow-off valve（1）And ball valve（5）, start vacuum pump（7）Carry out evacuation；
（2）, qualitative filter paper is laid in the bottom of buchner funnel, add appropriate water-wet simultaneously to make filter paper be close to buchner funnel bottom
Portion, opens ball valve, and in funnel, water closes ball valve when being filtered dry, and closes blow-off valve after opening the water that blow-off valve is discharged in bottle,suction；
（3）, black titanium liquid is heated to predetermined temperature and stirs after, pour buchner funnel into（2）Interior, open ball valve（5）Carry out
Vacuum filtration, in funnel, black titanium liquid closes ball valve when being filtered dry（5）, open blow-off valve（1）, extract the black titanium through a sucking filtration
Liquid.
3. detection method according to claim 1 it is characterised in that wherein step one（3）In small step, to through one
The filter mud that the black titanium liquid supplement of secondary sucking filtration is appropriate is obtained standard specimen black titanium liquid, and the addition of described filter mud is filtered according in black titanium liquid to be measured
Mud be determined containing concentration it is ensured that standard specimen black titanium liquid and black titanium liquid phase to be measured contain in vitro than eliminating water dispergation equal miscellaneous
Matter.
4. detection method according to claim 1 it is characterised in that wherein step 2（3）Black titanium to be measured in small step
The of the heating-up temperature of liquid and sucking filtration vacuum and step one（4）The heating-up temperature of standard specimen black titanium liquid and sucking filtration vacuum in small step
Corresponding consistent.
5. detection method according to claim 1 is it is characterised in that standard specimen in black titanium liquid to be measured and step one in step 2
Black titanium liquid is extracted from same production line source.
6. the detection method according to any one of claim 1-5 is it is characterised in that described ball valve in described detection means
（5）It is arranged at VRV（6）And safety flack（4）Between connecting line on, the bottleneck of described safety flack passes through to carry two-tube
The bottle stopper sealing on road.
7. the detection method according to any one of claim 1-5 is it is characterised in that described sucking filtration in described detection means
Bottle（3）For upper and lower mouth taper bottle,suction, in bottle,suction（3）Taper upper side wall on offer aspirating hole, described safety flack passes through
Connecting line is connected to described aspirating hole, in bottle,suction（3）Conical lower portion offer relief hole, described relief hole is connected with
Marker pipe, described marker pipe is provided with described blow-off valve（1）, the open top of described bottle,suction is by bottle stopper sealing even
It is connected to described buchner funnel（2）.
8. the detection method according to any one of claim 1-5 is it is characterised in that described Bu Shi in described detection means
Funnel is the buchner funnel of φ 80mm, and described bottle,suction is the taper bottle,suction of mouth up and down of 1000ml, by described vacuum pump（7）
And VRV（6）Described safety flack can be made（4）And bottle,suction（3）Interior vacuum is maintained at below -0.04Mpa.
9. in a kind of black titanium liquid acid hemolysis process of titanium white early stage hydrolysis degree detection method, described detection method is based on the black titanium of titanium white
In liquid acid hemolysis process, the detection means of early stage hydrolysis degree is carried out, and described detection means includes：Blow-off valve（1）, buchner funnel
（2）, bottle,suction（3）, safety flack（4）, ball valve（5）, VRV（6）, vacuum pump（7）And connecting line, described vacuum pump
（7）Vacuum orifice safety flack is connected to by connecting line（4）, and it is provided with ball valve on described connecting line（5）With true
Empty air relief valve（6）, described safety flack（4）Described bottle,suction is connected to by connecting line（3）, described buchner funnel（2）Install
In described bottle,suction（3）Bottleneck, described blow-off valve（1）It is arranged at described bottle,suction（3）Drainage line on, its feature exists
In described detection method comprises the following steps：
Step one, making standard specimen black titanium liquid, obtain the standard comparison time, specifically include：
（1）, take the black titanium liquid of 200ml on production line, add the activated carbon powder of 0.1g 325 mesh fully to adsorb hydrocolloid therein；
（2）, close blow-off valve（1）And ball valve（5）, start vacuum pump（7）, adjust VRV（6）So that vacuum-
0.04～-0.05Mpa；
（3）, two φ 70mm qualitative filter papers are entirely placed in the buchner funnel of φ 80mm（2）Bottom, adds 20ml water, opens
Ball valve（5）, when water is filtered dry, close ball valve（5）, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom, then open
Blow-off valve（1）Blow-off valve is closed after discharging the water in bottle,suction（1）；
（4）, by the black titanium liquid of above-mentioned 200ml, be heated to 68～70 DEG C, stir, pour buchner funnel into（2）, open ball valve
（5）Carry out sucking filtration, after titanium liquid sample black in funnel is drained, close ball valve（5）, open blow-off valve and extract after a sucking filtration
Black titanium liquid；
（5）, add 0.5g filter mud in the black titanium of the 200ml once liquid to above-mentioned sucking filtration, after stirring, extract 50ml black titanium liquid and make
For standard specimen black titanium liquid, and it is heated to 68～70 DEG C；
（6）, close blow-off valve（1）And ball valve（5）, start vacuum pump（7）, adjust VRV（6）So that vacuum-
0.04～-0.05Mpa；
（7）, the qualitative filter paper of two φ 70mm is entirely placed in the buchner funnel of φ 80mm（2）Bottom, adds 20ml water, opens
Open ball valve（5）, when water is filtered dry, close ball valve（5）, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom；
（8）, black for above-mentioned 50ml standard specimen titanium liquid is heated to 68～70 DEG C, stir, pour buchner funnel again into（2）, open
Ball valve（5）, adjust VRV（6）It is ensured that vacuum is in -0.04～-0.05Mpa, starts sucking filtration, and start timing；
（9）, treat buchner funnel（2）When interior standard specimen black titanium liquid is filtered dry, stop timing, close ball valve（5）, during the sucking filtration being recorded
Between as standard comparison time t0；
Step 2, extraction black titanium liquid to be measured, detect the sucking filtration time, specifically include：
（1）, close blow-off valve（1）And ball valve（5）, start vacuum pump（7）, adjust VRV（6）It is ensured that vacuum-
0.04～-0.05Mpa；
（2）, two φ 70mm qualitative filter papers are entirely placed in the buchner funnel of φ 80mm（2）Bottom, adds 20ml water, opens
Ball valve（5）, closing ball valve when water filter is drained（5）, qualitative filter paper is lubricated and tiles and be close to buchner funnel bottom；
（3）, on same production line extract 50ml black titanium liquid to be measured, be heated to 68～70 DEG C, stir, pour buchner funnel into
（2）Interior, open ball valve（5）, adjust VRV（6）It is ensured that vacuum is in -0.04～-0.05Mpa, starts sucking filtration, and open
Beginning timing；
（4）, treat buchner funnel（2）When interior to be measured black titanium liquid is filtered dry, stop timing, close ball valve（5）, the time used by record is
Sucking filtration time t1 for black titanium liquid to be measured；
The standard ratio of the standard specimen black titanium liquid that step 3, the to be measured black titanium liquid sucking filtration time t1 that step 2 is recorded and step one are demarcated
Time t0 is analyzed, the standard comparison time t0 of the sucking filtration time t1 based on black titanium liquid to be measured and standard specimen black titanium liquid it
Between departure degree judge black titanium liquid to be measured early stage hydrolysis degree.
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Inventor after: Deng Gang Inventor before: Pan Xianglei Inventor before: Yang Jiahua |