CN109490130A - A kind of determining saltcake solution is detained the method for speed by dynamic crystallization in filter - Google Patents
A kind of determining saltcake solution is detained the method for speed by dynamic crystallization in filter Download PDFInfo
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- CN109490130A CN109490130A CN201810813316.0A CN201810813316A CN109490130A CN 109490130 A CN109490130 A CN 109490130A CN 201810813316 A CN201810813316 A CN 201810813316A CN 109490130 A CN109490130 A CN 109490130A
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- saltcake
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
Abstract
The present invention provides a kind of determining saltcake solution to pass through the method for dynamic crystallization delay speed in filter.This method comprises: design cycle filtration experiment device；Preparation SN type particle prepares fill-type filter, produces saltcake saturated solution；Saltcake solution filtration experiment is carried out, the specific surface of single SN type particle is calculated, calculates the total volume of SN type particle, calculates total surface area, measurement saltcake solution is changed by filter solution density under different temperatures, and calculates the concentration of saltcake solution；Utilize the dissolution and crystallization theory and material balance principle of substance, quantitatively characterizing sodium chloride crystal speed and its calculation method to filter inner pore surface sodium chloride crystal thickness growth rate are established, sodium chloride crystal speed and filter inner pore surface sodium chloride crystal thickness growth rate are calculated.The present invention can exploit and purify the filter design of industry for saltcake and chocking-up degree evaluation provides theoretical direction and foundation, and scene is suitble to use.
Description
Technical field
The present invention relates to the exploitations of mirabilite ore and purification manufacture field to be more specifically related to a kind of determining saltcake solution
It is detained the method for speed by dynamic crystallization in filter.
Background technique
Saltcake (main component Na2SO4·10H2O it is) a kind of very extensive sulfate mineral of distribution, is Sulfates mineral
The processed refined crystalline solid of saltcake, is important chemical industry, light industry raw material, is widely used in chemical industry, light industry, spinning
It knits, more than 20 a industries such as building materials, medicine.In commercial mining, processing purification process, filtering is that one of those must ring for it
Section.But since the solubility of saltcake in water is affected by temperature serious (see attached drawing 1), under suitable condition,
Saltcake can crystallize precipitation, be trapped on the pore surface of filter interior (schematic diagram is shown in attached drawing 2), and it is small to reduce filter interior
Flowing duct aperture, filter can be blocked when extreme, strainability decline causes fault in production when serious.Wherein saltcake
It is the key parameter of prevention and evaluation strainability by the crystallization rate in filter.Therefore, it establishes saltcake and passes through filter
The fast determination method of crystallization rate and crystal thickness variation, exploitation and purification to mirabilite ore are machined with important theory significance
And application value.But lack in the prior art about mirabilite ore crystallization rate and in the growth of dielectric surface crystallization thickness
The research of speed.
Summary of the invention
It is an object of the invention to solve the insurmountable mirabilite ore crystallization rate of the prior art and in dielectric surface knot
The technical issues of growth rate of brilliant thickness, provides a kind of determining saltcake solution by dynamic crystallization in filter and is detained speed
Method.
The present invention is to be achieved through the following technical solutions: a kind of determining saltcake solution is detained by dynamic crystallization in filter
The method of speed, comprising the following steps:
Step S1: design cycle filtration experiment device.
The circulating filtration experimental provision includes saltcake solution control system, filtration system, sampling and measuring system and pipeline
System；
The saltcake solution control system includes insulating box 1, temperature sensor 1 and liquor box；The filtration system includes
Fill-type filter, insulating box 2, temperature sensor 1, inlet pressure transducer and outlet pressure sensor；The sampling and measuring
System includes sample bucket；Control valve 1, flow pump, control valve 2, control valve 3 and control valve are sequentially installed on the pipeline system
4。
Step S2: preparation SN type particle prepares fill-type filter, produces saltcake saturated solution.
The method for preparing SN type particle are as follows:
1. selection is suitble to the SN profile material of processing, it is processed into graininess, by multipass sort, rounding, obtains pack grain；
2. being impregnated before filter filling with circulating cleaning fluid under the conditions of industrial temperature, filtering out moisture, pack grain
It is placed in baking oven 10h drying.
The method for preparing fill-type filter are as follows: weigh the filter quality for the SN type grain packing in the balance
m1；Using the SN type grain packing filter, claim to obtain its gross mass m2；By SN type particle compacting in filter.
The method for producing saltcake saturated solution are as follows:
1. taking container with a scale, it is packed into distilled water, the volume of water is read by scale, is heated to 38 DEG C；
2. weighing saltcake powder, its quality m is recorded3, the side into distilled water is taken to add saltcake powder, the side of side stirring
Formula stops addition saltcake powder, weighs remaining saltcake powder, record its quality m when saltcake reaches saturation3, calculate molten
The saltcake quality of solution is m4-m3；
3. calculating the solubility of saltcake at such a temperature according to the saltcake quality of the volume of water and dissolution.
Step S3: carrying out saltcake solution filtration experiment, calculates the specific surface of single SN type particle, calculates the total of SN type particle
Volume calculates total surface area, and measurement saltcake solution is changed by filter solution density under different temperatures, and it is molten to calculate saltcake
The concentration of liquid.
Saltcake solution filtration experiment method described in the step S3 are as follows:
1. connecting flow switch pump, observing the connector, whether leak winds the connector for having leak with CF type sealing material
Connector screw thread, tightens connector；
2. opening insulating box 1 to switch, its temperature is set as 38 DEG C, is opened insulating box 2 and is switched, sets a temperature value T1DEG C,
The temperature that temperature sensor to two insulating boxs is shown is constant；
3. adjustment flow pump makes it keep constant flow q1, filter is cycled through, at interval of regular hour dt, from sampling
It is sampled in bucket, measures its saltcake solution density, and record, the saltcake solution after measurement is re-poured into liquid case；
4. being sequentially adjusted in different flow q2、q3、、、qn, time interval and corresponding solution density are recorded respectively；
5. change the temperature of insulating box 2, repeat it is described 3.-experimental procedure 4., until experiment terminates.
Step S4: using the dissolution and crystallization theory and material balance principle of substance, quantitatively characterizing sodium chloride crystal speed is established
Degree and its to the calculation method of filter inner pore surface sodium chloride crystal thickness growth rate, calculates sodium chloride crystal speed and filtering
Device inner pore surface sodium chloride crystal thickness growth rate.
The specific surface calculation formula of the single SN type particle are as follows:
The total volume of SN type particle can pass through the density p of SN type granuleSNIt calculates, the total volume of the SN type particle
Calculation formula are as follows:
The total surface area calculation formula of the SN type particle are as follows:
St=VtSv
Wherein: SvFor the specific surface of single SN type particle, m-1；α is specific surface compensation coefficient, zero dimension；D is that particle is straight
Diameter, m；VtFor the total volume of SN type particle, m3；m1For filter quality, kg；m2To fill SN type particle and filter gross mass,
kg；Δ m is the gross mass of SN type particle, kg；ρSNFor the density of SN type particle, kg/m3；StFor the total surface face of SN type particle
Product, m2。
The concentration calculation formula of the saltcake solution are as follows:
Wherein: Cs(x, t) is saltcake concentration, kg/m3；Cs0For filter inlet end saltcake concentration, kg/m3；X be space away from
From m；T is time, s；V is flow velocity, m/s；DsFor diffusion coefficient, m2/s；Erfc is error function, no unit；Become for centre
Amount, 1/m；ζSIt is detained velocity coeffficient, 1/s for nitre.
The sodium chloride crystal speed calculation formula are as follows:
Filter inner pore surface sodium chloride crystal thickness growth rate calculation formula are as follows:
Wherein: RMj,iFor sodium chloride crystal speed, kg/s；RMu,j,iFor the knot of saltcake on the filler particles surface of unit quality
Brilliant speed s-1；Hj,iFor the saltcake thickness growth rate of crystallization, m/s；VsFor the volume of saltcake solution, m3；Cj,i-1And Cj,iRespectively
It is T for temperaturejWhen the time be respectively ti-1And tiThe concentration kg/m of moment saltcake solution3；Δtj,iFor time interval, s；Δm0For
Unit mass, kg；ρSNFor the density of SN type particle, kg/m3；SvFor the specific surface of SN type particle, m-1；VtFor the total of SN type particle
Volume, m3。
The beneficial effects of the present invention are: devising circulating filtration experimental provision based on solution filtration experiment, realize
The real time measure of saltcake solution density under flow regime；Using saltcake solution by SN type packing models of filler, saltcake is simulated
Dynamic crystallization process in fill-type filter；Using the specific surface of pore media, the total pore space table of filling model is established
Area computation method；Using the dissolution and crystallization theory and material balance principle of saltcake, quantitatively characterizing sodium chloride crystal speed is established
And its calculation method to filter inner pore surface sodium chloride crystal thickness, it is suitble to field application.
Detailed description of the invention
Fig. 1 is the solubility curve of saltcake in water；
Fig. 2 is crystallization schematic diagram of the nitre on filler particles surface；(A) before for crystallization, (B) is after crystallizing
Fig. 3 is to determine that saltcake solution is detained the method flow schematic diagram of speed by dynamic crystallization in filter；
Fig. 4 is circulating filtration Experimental equipment
Specific embodiment
Below with reference to embodiment, invention is further described in detail, but embodiments of the present invention are not limited only to this.
Fig. 3 shows determining saltcake solution according to the present invention and passes through the method for dynamic crystallization delay speed in filter
Process.
As shown in figure 3, a kind of determining saltcake solution provided by the invention is detained speed by dynamic crystallization in filter
Method, comprising the following steps:
Step S1: design cycle filtration experiment device；
Step S2: preparation SN type particle prepares fill-type filter, produces saltcake saturated solution；
Step S3: carrying out saltcake solution filtration experiment, calculates the specific surface of single SN type particle, calculates the total of SN type particle
Volume calculates total surface area, and measurement saltcake solution is changed by filter solution density under different temperatures, and it is molten to calculate saltcake
The concentration of liquid；
Step S4: using the dissolution and crystallization theory and material balance principle of substance, quantitatively characterizing sodium chloride crystal speed is established
Degree and its to the calculation method of filter inner pore surface sodium chloride crystal thickness growth rate, calculates sodium chloride crystal speed and filtering
Device inner pore surface sodium chloride crystal thickness growth rate.
In order to make it easy to understand, the present invention is illustrated with a specific example.
1, circulating filtration experimental provision assembles
Saltcake solution control system, filtration system, sampling and measuring system and pipeline system are connected according to shown in attached drawing 4.
2, steps are as follows for specific experiment:
1) prepare SN type particle: selection is suitble to the SN profile material of processing, is processed into graininess, by multipass sort, rounding,
The pack grain of L mesh is obtained, corresponding partial size is D.It is soaked before filter filling with circulating cleaning fluid under the conditions of industrial temperature
Bubble, filters out moisture, and pack grain is placed in baking oven 10h drying.
2) it prepares fill-type filter: weighing the filter quality m for being taken as filling SN type particle in the balance1, using step 1)
The SN type particle of preparation fills filter, claims to obtain its quality m2。
3) it produces saltcake saturated solution: taking container with a scale, be packed into distilled water, the volume V of water is read by scale1,
It is heated to 38 DEG C (saltcake solubility is maximum when the temperature).Weigh saltcake powder m3, the side into distilled water is taken to add awns
Nitre powder, the mode of side stirring stop addition saltcake powder, weigh remaining saltcake powder, remember when saltcake reaches saturation
Recording its quality is m4；The saltcake quality then dissolved is m4-m3.According to the saltcake quality of the volume of water and dissolution, calculates saltcake and exist
Solubility at this temperature.
4) test leakproofness: connect flow switch pump, observe the connector whether leak, to the connector for having leak, with CF type
Sealing material winds connector screw thread, tightens connector.
5) experiment condition is set: being opened insulating box 1 and is switched, sets its temperature as 38 DEG C；It opens insulating box 2 to switch, setting
Its temperature is T1℃；The temperature that temperature sensor to two insulating boxs is shown is constant.
6) parameter measurement and record: adjustment flow pump makes it keep constant flow q1Filter is cycled through, when at interval of dt
Between after, from sample bucket sample, measure its saltcake solution density, and record, which be re-poured into liquid case.It is sequentially adjusted in flow
q2、q3、、、qn, time interval and corresponding solution density are recorded respectively.
7) step 5) is returned to, the temperature of insulating box 2 is changed, repeats step 6), until experiment terminates.
3, calculation method
1) specific surface of the filler particles based on skeleton volume calculates: since the SN type particle of use is by special disposal
The preferable almost spherical of sorting grain packing, intergranular is particle point contact, and spheric granules fills the specific grain surface of model
According to definition, it is assumed that the granule number filled in unit volume is n, be can be expressed as:
2) total surface area of filler particles calculates: calculating the gross mass for filter SN type particle are as follows:
Δ m=m2-m1
The total volume of all SN type particles can pass through the volume density ρ of particleSNIt calculates:
The total surface area calculation formula of all SN type particles in filter are as follows:
St=VtSv
Wherein: SvFor the specific surface of single SN type particle, m-1；α is specific surface compensation coefficient, zero dimension；D is that particle is straight
Diameter, m；VtFor the total volume of SN type particle, m3；m1For filter quality, kg；m2To fill SN type particle and filter gross mass,
kg；Δ m is the gross mass of SN type particle, kg；ρSNFor the density of SN type particle, kg/m3；
StFor the total surface area of SN type particle, m2。
3) filter interior solution concentration governing equation and solution:
Primary condition are as follows:
Cs=Cs0
It is using the concentration that Laplace transformation technology acquires saltcake solution
Wherein: Cs(x, t) is saltcake concentration, kg/m3；Cs0For filter inlet end saltcake concentration, kg/m3；X be space away from
From m；T is time, s；V is flow velocity, m/s；DsFor diffusion coefficient, m2/s；；Erfc is error function, no unit；Become for centre
Amount, 1/m；ζSIt is detained velocity coeffficient, 1/s for nitre.
The saltcake solution concentration of entire experiment outlet end and entrance can regard approximately equal as, that is to say, that, it is believed that mistake
Inside filter at a time, saltcake solution concentration does not change along flow direction, only the function of time.
4) sodium chloride crystal speed calculates:
Record time interval Δ t at a certain temperaturej,iThe density of front and back saltcake solution is respectively ρj,i-1And ρj,i, respectively correspond
Concentration be respectively Cj,i-1And Cj,i.The volume V of known saltcake solutions, then interval of delta tj,iCrystallization of the interior saltcake in filter
Quality are as follows:
Mj,i=Vs(Cj,i-Cj,i-1)
The mass velocity of filter interior sodium chloride crystal is
The crystallization rate of saltcake on the filler particles surface of unit mass are as follows:
5) sodium chloride crystal thickness speed calculates: according to the quality crystalline speed, saltcake crystalline density and pack grain of saltcake
Total surface area, approximate can acquire crystallization thickness growth rate of the saltcake on filler particles surface are as follows:
Wherein: RMj,iFor sodium chloride crystal speed, kg/s；RMu,j,iFor the knot of saltcake on the filler particles surface of unit quality
Brilliant speed s-1；Hj,iFor the saltcake thickness growth rate of crystallization, m/s；VsFor the volume of saltcake solution, m3；Cj,i-1And Cj,iRespectively
It is T for temperaturejWhen the time be respectively ti-1And tiThe concentration kg/m of moment saltcake solution3；Δtj,iFor time interval, s；Δm0For
Unit mass, kg；ρSNFor the density of SN type particle, kg/m3；SvFor the specific surface of SN type particle, m-1；VtFor the total of SN type particle
Volume, m3。
6) example and result
Using method of the invention, saltcake solution has been obtained under the conditions of crystallization temperature is 25 and 30 DEG C by moving in filter
State crystallization rate, by the mass velocity and crystallization thickness growth rate parameter characterization sodium chloride crystal speed that crystallize saltcake.It is used
Basic parameter be shown in Table 1.
1 basic parameter table of table
| Test basic parameter title and unit | Numerical value |
| SN grain density (g/cm3) | 2.623 |
| Saltcake crystalline density (g/cm3) | 1.481 |
| Saltcake liquor capacity, cm3 | 1000.000 |
| Receiving volume in cylindrical filter, cm3 | 200.000 |
| Cylindrical filter cross-sectional area, cm2 | 10.000 |
| Cylindrical filter length, cm | 20.000 |
| Pack grain SN skeleton volume, cm in filter3 | 128.500 |
| Filler particles partial size cm | 0.015 |
| Filler particles specific surface area, m-1 | 480.000 |
(note: in order to be suitble to calculating and Data Processing in Experiment, length uses cm；Area uses cm2；Volume uses
cm3；Quality uses g；Time uses min.Unit conversion relationship in formula in the present invention: 1m=100cm；1min=60s；
1kg=1000g)
25 have been obtained using basic parameter shown in table 1 using the method for quantitatively determining sodium chloride crystal speed of the invention
DEG C and 30 DEG C under the conditions of saltcake solution by dynamic crystallization speed in filter, be shown in Table 2.
2 the actual calculation table of table
The above, be only presently preferred embodiments of the present invention not to the present invention to limitation in any form, it is all according to
According to any simple modification, equivalent variations made by technology of the invention, the substantial above embodiments of method, each fall within of the invention
Within protection scope.
Claims (10)
1. a kind of determining saltcake solution is detained the method for speed by dynamic crystallization in filter, which is characterized in that including following
Step:
Step S1: design cycle filtration experiment device；
Step S2: preparation SN type particle prepares fill-type filter, produces saltcake saturated solution；
Step S3: carrying out saltcake solution filtration experiment, calculates the specific surface of single SN type particle, calculates the totality of SN type particle
Product calculates total surface area, and measurement saltcake solution is changed by filter solution density under different temperatures, and calculates saltcake solution
Concentration；
Step S4: using substance dissolution and crystallization theory and material balance principle, establish quantitatively characterizing sodium chloride crystal speed and
Its calculation method to filter inner pore surface sodium chloride crystal thickness growth rate calculates in sodium chloride crystal speed and filter
Pore surface sodium chloride crystal thickness growth rate.
2. determining saltcake solution according to claim 1 is detained the method for speed by dynamic crystallization in filter, special
Sign is: the circulating filtration experimental provision includes saltcake solution control system, filtration system, sampling and measuring system and pipeline system
System.
3. determining saltcake solution according to claim 2 is detained the method for speed by dynamic crystallization in filter, special
Sign is: the saltcake solution control system includes insulating box 1, temperature sensor 1 and liquor box；The filtration system includes filling
Fill out formula filter, insulating box 2, temperature sensor 1, inlet pressure transducer and outlet pressure sensor；The sampling and measuring system
System includes sample bucket；Control valve 1, flow pump, control valve 2, control valve 3 and control valve 4 are sequentially installed on the pipeline system.
4. determining saltcake solution according to claim 3 is detained the method for speed by dynamic crystallization in filter, special
Sign is: the method for SN type particle is prepared described in the step S2 are as follows:
1. selection is suitble to the SN profile material of processing, it is processed into graininess, by multipass sort, rounding, obtains pack grain；
2. being impregnated before filter filling with circulating cleaning fluid under the conditions of industrial temperature, filtering out moisture, pack grain is placed in
Baking oven 10h drying.
5. determining saltcake solution according to claim 4 is detained the method for speed by dynamic crystallization in filter, special
Sign is: the method for fill-type filter is prepared described in the step S2 are as follows: weighs in the balance for the SN type grain packing
Filter quality；Using the SN type grain packing filter, claim to obtain its gross mass；SN type particle compacting is being filtered
In device.
6. determining saltcake solution according to claim 5 is detained the method for speed by dynamic crystallization in filter, special
Sign is: the method for saltcake saturated solution is produced described in the step S2 are as follows:
1. taking container with a scale, it is packed into distilled water, the volume of water is read by scale, is heated to 38 DEG C；
2. weighing saltcake powder, its quality is recorded, side is taken into distilled water to add saltcake powder, the mode of side stirring, until
When saltcake reaches saturation, stops addition saltcake powder, weigh remaining saltcake powder, record its quality, calculate the saltcake of dissolution
Quality；
3. calculating the solubility of saltcake at such a temperature according to the saltcake quality of the volume of water and dissolution.
7. determining saltcake solution according to claim 6 is detained the method for speed by dynamic crystallization in filter, special
Sign is: saltcake solution filtration experiment method described in the step S3 are as follows:
1. connecting flow switch pump, observing the connector, whether leak winds connector with CF type sealing material to the connector for having leak
Screw thread tightens connector；
2. opening insulating box 1 to switch, its temperature is set as 38 DEG C, is opened insulating box 2 and is switched, a temperature value is set, to two perseverances
The temperature that the temperature sensor of incubator is shown is constant；
3. adjustment flow pump makes it keep constant flow, filter is cycled through, at interval of the regular hour, is taken from sample bucket
Sample measures its saltcake solution density, and records, and the saltcake solution after measurement is re-poured into the liquor box；
4. being sequentially adjusted in different flows, time interval and corresponding solution density are recorded respectively；
5. change the temperature of insulating box 2, repeat it is described 3.-experimental procedure 4., until experiment terminates.
8. determining saltcake solution according to claim 7 is detained the method for speed by dynamic crystallization in filter,
It is characterized in that: the specific surface calculation formula of single SN type particle described in the step S3 are as follows:
The total volume calculation formula of the SN type particle are as follows:
Δ m=m2-m1
The total surface area calculation formula of the SN type particle are as follows:
St=VtSv
Wherein: SvFor the specific surface of single SN type particle, m-1；α is specific surface compensation coefficient, zero dimension；D is particle diameter, m；Vt
For the total volume of SN type particle, m3；m1For filter quality, kg；m2For filling SN type particle and filter gross mass, kg；Δm
For the gross mass of SN type particle, kg；ρSNFor the density of SN type particle, kg/m3；StFor the total surface area of SN type particle, m2。
9. determining saltcake solution according to claim 8 is detained the method for speed by dynamic crystallization in filter, special
Sign is: the concentration calculation formula of saltcake solution described in the step S3 are as follows:
Wherein: Cs(x, t) is saltcake concentration, kg/m3；Cs0For filter inlet end saltcake concentration, kg/m3；X is space length, m；
T is time, s；V is flow velocity, m/s；DsFor diffusion coefficient, m2/s；Erfc is error function, no unit；θ is intermediate variable, 1/m；
ζSIt is detained velocity coeffficient, 1/s for nitre.
10. determining saltcake solution according to claim 9 is detained the method for speed by dynamic crystallization in filter, special
Sign is: the sodium chloride crystal speed calculation formula are as follows:
The crystallization rate of saltcake on the filler particles surface of unit mass are as follows:
Filter inner pore surface sodium chloride crystal thickness growth rate calculation formula are as follows:
Wherein: RMj,iFor sodium chloride crystal speed, kg/s；RMu,j,iFor the crystallization speed of saltcake on the filler particles surface of unit quality
Spend s-1；Hj,iFor the saltcake thickness growth rate of crystallization, m/s；VsFor the volume of saltcake solution, m3；Cj,i-1And Cj,iIt is respectively warm
Degree is TjWhen the time be respectively ti-1And tiThe concentration kg/m of moment saltcake solution3；Δtj,iFor time interval, s；Δm0For unit
Quality, kg；ρSNFor the density of SN type particle, kg/m3；SvFor the specific surface of SN type particle, m-1；VtFor the totality of SN type particle
Product, m3。
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