CN104155338B - Method for measuring bound water content in sludge - Google Patents
Method for measuring bound water content in sludge Download PDFInfo
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- CN104155338B CN104155338B CN201410441816.8A CN201410441816A CN104155338B CN 104155338 B CN104155338 B CN 104155338B CN 201410441816 A CN201410441816 A CN 201410441816A CN 104155338 B CN104155338 B CN 104155338B
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Abstract
The invention discloses a method for measuring bound water content in sludge, and belongs to the field of characterization of a water index in the sludge. The method comprises the following steps: measuring spectral characteristics of different types of moistures of a simulated material; putting a sludge sample into an environment of which the temperature can be changed, and measuring heat absorbed or released during form transformation of the sludge sample by using a differential scanning calorimeter; performing thermal analysis on the measured heat to obtain a thermal analysis spectrum, and calculating the peak area of an exothermic peak in the thermal analysis spectrum to obtain condensation heat of the sludge sample; calculating the bound water content in the sludge sample by virtue of the condensation heat. By the method, the bound water content in the sludge can be accurately measured.
Description
Technical field
The present invention relates to moisture percentage in sewage sludge fields of measurement, the method that more particularly to a kind of measurement mud combines water content.
Background technology
Mud is sewage disposal final product, is a kind of heterogeneous body, mainly by organic relic, microorganism, inorganic particulate
Grain, colloid etc. form, and its composition is extremely complex.In mud, contained humidity can be divided into four classes：Free water, Interstitial Water, surface water
With combine water.Wherein Free water, not with any form and mud attachment or combination, accounts for the 70% of sludge water content, available gravity divides
From；Interstitial Water is the water keeping because of capillarity between mud, and the available mechanical force such as centrifugation, vacuum makes particle deformation, compression
And separate；Surface water is the water molecule layer being attached to colloid surface by hydrogen bond, only could mechanically take off through conditioning
Water removes；Refer to the water combined closely by chemical bond and mud in conjunction with water, account for the 4% of sludge water content.By domestic and international
The investigation of research conditions, it is known that the distribution situation of mud unfree water directly affects the complexity of sludge dewatering, therefore, is carried out
The research of sludge dewatering characteristic particularly moisture distribution is very necessary.
Various moisture contained by from mud flco are not difficult to find out, combine the content of water for sludge dewatering characteristic in mud
For be also an important indicator, the complexity of sludge dewatering can be characterized in terms of moisture distribution, thus reaching table
Levy the purpose of sludge dewatering characteristic.
Characterizing method in conjunction with water has a lot, and conventional method mainly includes heated drying method, dilatometric method, TG-DTA
Analytic process (TG-DTA), suction method and water activity method etc..But how to be more convenient, accurately measure the content with reference to water in mud be
The problem needing to solve.
Content of the invention
Based on the problems of above-mentioned prior art, the present invention provides one kind can be more convenient accurately to measure combination in mud
The method of water content, solves existing method measurement and combines that water is inconvenient or inaccurate problem.
For solving above-mentioned technical problem, the present invention provides a kind of method that measurement mud combines water content, can be first using mould
Intend material, obtain chromatogram characteristic and the thermal change rule of dissimilar moisture；
Mud sample is placed in the environment that can change temperature, described mud sample is recorded using differential scanning calorimeter and exists
The heat absorbing during form transformation or discharging；
Heat analysis are carried out to the described heat recording and obtains heat analysis collection of illustrative plates, by described heat analysis collection of illustrative plates and the simulation recording
The chromatogram characteristic of the dissimilar moisture of material is contrasted, and calculates exothermic peak peak area in described heat analysis collection of illustrative plates and obtain institute
State the heat of condensation of mud sample；
It is calculated the combination water content of described mud sample using the described heat of condensation.
Beneficial effects of the present invention are：The thermal effect that the method produces to mud sample should be able to provide due compensation in time,
Make in the no temperature difference, no heat exchange state between mud sample and reference substance, mud sample programming rate follows environment temperature all the time
Degree is linear to heat up, so that measurement sensitivity and precision greatly improve.
Brief description
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be to required use in embodiment description
Accompanying drawing be briefly described it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is measuring method schematic flow sheet provided in an embodiment of the present invention；
Fig. 2 is the thermal analysis curue of mud after the drying that measuring method provided in an embodiment of the present invention measures；
Fig. 3 is the thermal analysis curue of the mud sample of measuring method measurement provided in an embodiment of the present invention.
Specific embodiment
Below the embodiment it is clear that described is clearly and completely described to the technical scheme in the embodiment of the present invention
It is only a part of embodiment of the present invention, rather than whole embodiments.Based on embodiments of the invention, ordinary skill
The every other embodiment that personnel are obtained under the premise of not making creative work, broadly falls into protection scope of the present invention.
The embodiment of the present invention provides a kind of method that measurement mud combines water content, can accurately measure mud and combine water
Content, the method is as shown in figure 1, comprise the following steps：
Record the chromatogram characteristic of the dissimilar moisture of simulation material；
Mud sample is placed in the environment that can change temperature, heat flow flux type (can be adopted using differential scanning calorimeter DSC
DSC) record the heat that described mud sample absorbs in form transformation or discharges；
Carry out heat analysis using the described heat recording and obtain heat analysis collection of illustrative plates, by described heat analysis collection of illustrative plates and described simulation
The chromatogram characteristic of the dissimilar moisture of material is contrasted, and calculates exothermic peak peak area in described heat analysis collection of illustrative plates and obtain institute
State the heat of condensation of mud sample；
It is calculated the combination water content of described mud sample using the described heat of condensation.
In said method, calculate the heat of condensation that exothermic peak peak area in described heat analysis collection of illustrative plates obtains described mud sample,
Exothermic peak peak area in heat analysis collection of illustrative plates can be calculated by following formula (1)：
In above-mentioned formula (1), △ HFUSThe heat of condensation for mud sample；Q is the heat release (W/g) of every gram of mud；β is cooling
Speed；T1And T2It is respectively the temperature at peak two ends.
In said method, it is calculated the combination water content of described mud sample using the described heat of condensation, can be by following public affairs
Formula (2) is calculated the combination water content of mud sample：
In above-mentioned formula (2), ωsFor moisture percentage in sewage sludge (%)；WbIt is with reference to water content (kg/kg DS)；△HFUSFor mud
The heat of condensation (J/g) of sample.
In said method, described mud sample is recorded using differential scanning calorimeter and absorbs in form transformation or discharge
Heat be：Atmosphere during measurement is N2Atmosphere, gas flow rate is 50mL/min, rises or rate of temperature fall is 2 DEG C/min, will measure
Mud sample be first down to -80 DEG C and go up again to assigned temperature, measure mud sample and absorb in form transformation or discharge
Heat.
In said method, the chromatogram characteristic of the dissimilar moisture of simulation material is recorded using differential scanning calorimeter, main
If in order to obtain dissimilar moisture whether appearance and go out peak position, as long as there being appearance all can calculate the heat of condensation, simulating material
For in soil, milk, glucose solution one or more.
In said method, mud sample is the dry mud after dehydration and/or the mud sample after different microwave conditioning.
With reference to specific embodiment, the method for the present invention is described further.
Present invention method use be heat flow flux type DSC, dsc measurement be temperature and hot-fluid relation, this with dirt
The heat deflection of mud sample interior is related, and the method first records the chromatogram characteristic of the dissimilar moisture of simulation material, by mud sample
Product are placed in controlled environment and change temperature, the heat absorbing during determination sample form transformation (water-ice conversion) or discharging,
Directly carry out heat analysis, according to not freezing at a certain temperature with reference to water it is assumed that and being discharged during form transformation in sample
Heat is directly proportional to free water content in sample.
Concrete steps：
Uniformly the sample of about 5mg to 10mg is taken to put into specific aluminum cup after mud sample (can directly obtain)
Interior, cover crucible cover, carry out punching press film-making with crimping suppressor.Degasification is external, solid, liquid or thick sample
For measuring.Sample should be made during dress sample as far as possible uniformly, to be densely distributed in sample crucible, to improve heat transfer efficiency, reduce heat
Resistance.
Atmosphere during measurement is N2Atmosphere, gas flow rate is 50mL/min, heats up or rate of temperature fall is 2 DEG C/min, sample
First it is down to -80 DEG C to go up to assigned temperature, with the hot-fluid situation of this observed and recorded sample again.
When choosing soil simulation property DSC experiment, fetched earth earth records moisture content and is about 10%, takes after soil sample is dried
Sample is tested, and moisture content is 20%, 30%, 40%, 50% soil sample enters respectively to add quantitative water to be configured to in soil sample
Row test.
Plain chocolate and skim milk are carried out contrast experiment.Plain chocolate composition is：Protein 3.0%, fat 3.6%, carbon
Hydrate 4.5%, sodium 0.06%, calcium 0.1%, non-fat solid >=8.1%.Skim milk composition is：Protein 3.0%,
Carbohydrate 5.1%, sodium 0.058%, food additive.
Prepare the glucose solution of variable concentrations with glucose powder and pure water, the glucose concentration of preparation is 5%,
10%th, 20%, 30%, and carry out DSC test respectively.
Glucose powder and plain chocolate are 1 according to mass ratio：3、1：4、1：5、1：6 ratio carries out sample preparation, then
Carry out DSC test.
The mud that moisture content after dehydration is 86.05% is carried out gradual drying, that is, during to drying sludge, when
Detect the moisture that sample loses account for bulk sample 45% when stop being dried and sampling and testing, same mode in moisture content is
55%th, 65%, 75% when carry out, gained DSC heat analysis collection of illustrative plates as Fig. 2 be dried after mud thermal analysis curue.
Fig. 3 is the thermal analysis curue of mud, and sample represents respectively, process time correspond to 30s, 60s, 120s, 180s,
240s, carries out DSC heat analysis through five samples that the microwave for 600W for the power nurses one's health mud.Each conditioning condition of gained will be analyzed
The heat of condensation of lower mud is converted.Exothermic peak integrating peak areas in gained heat analysis collection of illustrative plates will be tested, peak area is this examination
The heat of condensation of sample, as formula (1)：
In above formula, q is the heat release (W/g) of every gram of mud；β is rate of temperature fall；T1And T2It is respectively the temperature at peak two ends.Change
During calculation, the heat of condensation of pure water is 334.7J/g.In conjunction with water content WbAs formula (2) is converted：
In above formula, ωsFor moisture percentage in sewage sludge (%)；WbIt is with reference to water content (kg/kg DS)；△HFUSFor the sample heat of condensation
(J/g).
Calculate and be recorded in table 1 with reference to water content by formula (1), formula (2).
Water content is combined under table 1 different condition
By upper table as can be seen that can accurately measure, using the method for the present invention, the content that mud combines water, by other
Factor impact is less, improves certainty of measurement.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, the change or replacement that can readily occur in,
All should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (5)
1. a kind of measurement mud combines the method for water content it is characterised in that including：
Record the chromatogram characteristic of the dissimilar moisture of simulation material；
Mud sample is placed in the environment that can change temperature, described mud sample is recorded in form using differential scanning calorimeter
The heat absorbing during conversion or discharging；
Heat analysis are carried out to the described heat recording and obtains heat analysis collection of illustrative plates, by described heat analysis collection of illustrative plates and the described simulation recording
The chromatogram characteristic of the dissimilar moisture of material is contrasted, and calculates exothermic peak peak area in described heat analysis collection of illustrative plates and obtain institute
State the heat of condensation of mud sample；
It is calculated the combination water content of described mud sample using the described heat of condensation.
2. according to claim 1 a kind of measurement mud combine water content method it is characterised in that described by mud sample
Product are placed in the environment that can change temperature, using differential scanning calorimeter record described mud sample absorb in form transformation or
Person release heat be：
Atmosphere during measurement is N2Atmosphere, gas flow rate is 50mL/min, rises or rate of temperature fall is 2 DEG C/min, by described in measurement
Mud sample is first down to -80 DEG C and is gone up to assigned temperature again, records described mud sample and absorbs in form transformation or discharge
Heat.
3. a kind of measurement mud according to claim 2 combines the method for water content it is characterised in that described mud sample
Form transformation be water-ice conversion.
4. a kind of measurement mud according to any one of claims 1 to 3 combines the method for water content it is characterised in that institute
Stating simulation material is：In soil, milk, glucose solution, milk and glucose mixed solution one or more.
5. a kind of measurement mud according to claim 1 combines the method for water content it is characterised in that described mud sample
For the dry mud after dehydration and/or the mud sample after different microwave conditioning.
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| CN201410441816.8A CN104155338B (en) | 2014-09-01 | 2014-09-01 | Method for measuring bound water content in sludge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104655675A (en) * | 2015-02-12 | 2015-05-27 | 北京市农林科学院 | Method for rapidly measuring content of unbound water |
| CN107817262A (en) * | 2017-10-24 | 2018-03-20 | 西南石油大学 | A kind of method based on low-field nuclear magnetic resonance appraisal drilling liquid surface hydration inhibitor |
| CN109030555A (en) * | 2018-08-17 | 2018-12-18 | 内蒙古蒙牛乳业（集团）股份有限公司 | A kind of test method of gel moisture holding capacity |
| CN109164007A (en) * | 2018-10-23 | 2019-01-08 | 桂林理工大学 | Volumetric flask surveys in soil the solution for combining its precision problem of water |
| CN109725022A (en) * | 2018-12-27 | 2019-05-07 | 湖南科技大学 | A kind of method for fast measuring of combination water content |
| CN111537553A (en) * | 2020-03-18 | 2020-08-14 | 浙江大学 | Method for rapidly determining free water ratio of floc sludge and granular sludge |
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| JPS5660698A (en) * | 1979-10-23 | 1981-05-25 | Ebara Infilco Co Ltd | Moisture estimation method of mechanically dehydrated cake of sludge |
| JPS62225950A (en) * | 1986-03-27 | 1987-10-03 | Inoue Japax Res Inc | Water content measuring apparatus for sludge |
| CN102628784A (en) * | 2012-04-13 | 2012-08-08 | 东华大学 | Form and content measuring device for industrial or urban sewage-sludge combined water |
| CN103308552B (en) * | 2013-06-17 | 2015-04-29 | 浙江大学 | Water comprehensive characterization method for oil-containing sludge |
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