CN103454180A - Method for measuring surface activation degree of modified powder material - Google Patents
Method for measuring surface activation degree of modified powder material Download PDFInfo
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Abstract
The invention provides a method for measuring the surface activation degree of a modified powder material. The method comprises the steps: adding water and an over dry modified powder material with a ratio of material to liquid of 0.02-0.05g/mL in a container, and standing after shaking; then adding liquid paraffin in the container according to the volume ratio of the liquid paraffin to the water of 1:(1-4), and standing until a water phase and an oil phase in the container demix after shaking; separating the water phase from the oil phase, and drying the modified powder material in the water phase to constant weight; and finally, calculating an activation index H of the modified powder material. According to the method, by using change of surface hydrophilicity and hydrophobicity before and after the powder material is modified, powder materials which are modified by a modifying agent and not modified by the modifying agent are dispersed in the water phase and the oil phase respectively for realizing separation, and thus the activation index is calculated. Compared with a conventional method for measuring the activation index, the method has the advantages that by using a water-oil two-phase measuring system, the applicable range is greatly widened, and the reliability and stability of a measurement result are improved.
Description
Technical field
The present invention relates to a kind of method that characterizes powder-modified effect, particularly a kind of method of measuring modified powder material degree of surface activation.
Background technology
The evaluation of modified effect is the important content of powder surface modification, seeks a kind of simple, reliable characterizing method, and the corresponding relation of setting up between modified technique parameter and quality index is significant concerning the research of powder material surface modification.At present, for the method that characterizes the powder material surface modification effect, have a variety of, as surface contact angle, surface energy, clad ratio, specific surface area, subsidence rate, oil absorption, water-intake rate and the activation index etc. of measuring powder.The activation index of wherein measuring modified powder is a kind of very quick, practical method of examining the quality of the production, in production using a quality index of its powder such as inorganic active filler after surface modification.Its principle is that powder material has a lot of polar groups to show as water wettability at the modification front surface, natural subsidence in water; Powder material surface after modification is become nonpolar by polarity, stronger hydrophobicity is arranged.The fine particle of this non-infiltration due to huge surface tension, swims on the water surface it in water.The number percent of the sample quality floated on the surface and sample gross mass is activation index.
The single-phase activation index measurement of traditional water system has significant limitation.One, the method by water to the surface tension of hydrophobic modified powder by being separated with unmodified powder granule of modification, the scope of application of this measuring method is little.The surface configuration that contains more impurity, powder in powder is irregular, the proportion of powder granule or size be when larger, water is not enough to overcome the gravity of himself to the surface tension of modified powder, modified powder also can sink down into the bottom, mix with unmodified powder, do not reach the purpose of measuring its activation index.Its two, it is extremely unstable in water that surface is hydrophobic modified powder, for reducing its surface free energy powder, easily reunites, along with the prolongation of time of repose, some agglomerated particle can sink under water, and affects stability and the accuracy of measurement result.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method of measuring modified powder material degree of surface activation is provided, the method has improved the reliability and stability of measurement result, and the scope of application is more extensive.
In order to achieve the above object, the technical solution used in the present invention comprises the following steps:
1) first water is joined in container, then the modified powder material of over dry is joined in container, wherein the modified powder material is that powder material by surface hydrophilicity is modified after the agent modification and obtains, the solid-liquid ratio of modified powder material and water is 0.02～0.05g/mL, by seal of vessel concussion, the powder material surface that the agent that makes in the modified powder material not to be modified is modified is by water-wet, then standing;
2) add whiteruss again in container, then by seal of vessel concussion, the powder material that the agent that makes in the modified powder material to be modified is modified enters the oil phase consisted of whiteruss, the powder material that simultaneously makes surface be modified by the agent that is not modified of water-wet enters water, more standing water and oil phase layering to container; The volume ratio of the water added in the whiteruss wherein added and step 1) is 1:(1～4);
3) by water and separation of oil, and will enter the powder material that the agent that is not modified in water modifies and be dried to constant weight;
4) press the activation index H that formula (1) calculates the modified powder material:
Wherein: m
1the dried quality of powder material for the agent modification that is not modified in step 3); The quality that m is the modified powder material that adds in step 1).
Powder material in described step 1) is the powder that calcium carbonate, silicon dioxide, titania or industrial sludge form.
Modifier in described step 1) is neopelex, stearic acid, maleic anhydride polyacrylate, Silane coupling agent KH550, odium stearate, titanate esters NDZ311, titanate esters NDZ401 or titanate esters NDZ311W.
The be modified concrete steps of agent modification of described powder material are: powder material is made into to the suspending liquid that mass concentration is 8～12%, add thermal agitation, dropwise add the dilution of modifier under 80～90 ℃, wherein the quality of modifier is 1～5% of powder material quality, filtration while hot after continuation stir process 60min, dry, grinding, sieve and obtain the modified powder material.
The particle diameter of described modified powder material is 1nm～250 μ m.
The modified powder material of the over dry in described step 1) obtains after cooling 30min after the modified powder material is dried to 4h under 100～110 ℃ in silica gel drier.
Concussion in described step 1) is for up and down reciprocatingly shaking 60～120 times; Time of repose is 30s.
Described whiteruss is chemical pure, and its principal ingredient is C
16～C
20n-alkane, density is 0.86～0.905.
Described step 2) concussion in is for up and down reciprocatingly shaking 90～150 times; Time of repose is 30min.
The concrete operations that the powder material that the agent that will not be modified in described step 3) is modified is dried to constant weight are that powder material that the agent that is not modified in water is modified is first put in advance the crucible type filtrator elimination moisture 100～110 ℃ of lower constant weights, be placed in again electric heating constant-temperature blowing drying box, under 100～110 ℃, be dried to constant weight.
Compared with prior art, the present invention has following beneficial effect:
The present invention first adds the modified powder material in water, can make to be adsorbed on by the mechanical oscillation effect modifier generation desorption that modified powder material surface not yet reacts, make the powder material that is the hydrophilic agent modification that is not modified by water-wet, enter water; Then to annex solution paraffin body in container, can form the compound three-phase froth system of whiteruss, modified powder material and air in oscillatory process, the powder material that the hydrophobic agent that is modified is modified is easy to be adsorbed on the gas/liquid interface of the surface of the whiteruss emulsion droplets in compound three-phase froth system and air/liquid paraffin bubble chamber film, and with water, separate in standing process, enter oil phase, i.e. the whiteruss phase.The present invention is by adopting this water-oil (whiteruss) two-phase to measure system, greatly expanded the measurement range of activation index, the 1nm of the particle diameter of measurable modified powder material when being measured by the single-phase measurement system of existing water～18 μ m expand 1nm～250 μ m to, have expanded the scope of application of the present invention; And the powder material surface that the agent that is modified is modified is coated with non-polar group, stronger lipophilicity (hydrophobicity) is arranged, in oil phase (whiteruss), can stable dispersion can not reunite, the error effect that simultaneously the present invention has avoided moisture to cause when calculating activation index as far as possible, improved the reliability and stability of measurement result.
Further, the present invention is not only applicable to the purer inorganic particles of component such as calcium carbonate, silicon dioxide, titania are carried out the measurement of its modified product degree of surface activation after modification, and can carry out the measurement of its modified product degree of surface activation after modification for the formed powder of the industrial sludge to complicated component, make the scope of application of the present invention more extensive.
The accompanying drawing explanation
Fig. 1 is determinator schematic diagram of the present invention;
Fig. 2 is measuring principle schematic diagram of the present invention;
Fig. 3 is stearic FI-IR figure;
Fig. 4 is the FI-IR figure of different mud powder, wherein a be blank mud powder, b be activation index be 56% stearic acid modified after mud powder, c be activation index be 100% stearic acid modified after the mud powder;
Fig. 5 is the TG figure of blank mud powder, and wherein a is the mass change curve, and b is the mass change rate curve;
Fig. 6 be activation index be 56% stearic acid modified after the TG figure of mud powder, wherein a is the mass change curve, b is the mass change rate curve;
Fig. 7 be activation index be 100% stearic acid modified after the TG figure of mud powder, wherein a is the mass change curve, b is the mass change rate curve;
Wherein: 1 is container, 2 is oil phase, 3 powder materials for the agent modification that is modified, 4 is water, 5 powder materials for the agent modification that is not modified, 6 hydrophilic groups that are modifier, 7 hydrophobic groups that are modifier, 8 for adding machinery concussion after water, 9 powder materials for the agent modification that is modified after the modifier of removing surperficial not absorption, 10 powder materials for the agent modification that is not modified by water-wet, 11 for adding machinery concussion after whiteruss, 12 is whiteruss emulsion droplets or air/liquid paraffin bubble.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Referring to Fig. 1, the present invention first joins water in container (pear shape separatory funnel) 1 and to form water 4, then the modified powder material is joined in container 1, and container 1 seal and shakes, and the powder material 5 of the agent modification that makes not to be modified enters in water 4; Then in container 1, add whiteruss as oil phase 2, then container 1 is sealed and shakes, the powder material 3 that the agent that makes to be modified is modified enters in oil phase 2, more standing water 4 and oil phase 2 layerings to container, because whiteruss density ratio water is little, so oil phase 2 is positioned at the top of water 4; Finally isolate water and dry the unmodified powder material in water, weigh, for the calculated activity index.
Referring to Fig. 2, the principle that water of the present invention-oil (whiteruss) two-phase measurement system is measured activation index is, modified powder material (powder material 5 that comprises the be modified powder material 3 of agent modification and the agent that is not modified modification) is added to water to be shaken, the polar group on powder material 3 surfaces that the agent that is modified is modified and hydrophilic group 6 combinations of modifier, the powder material 3 that the hydrophobic group 7 of modifier makes the agent that is modified modify becomes hydrophobicity by water wettability, and powder material 5 surfaces that the agent that is not modified is modified are water wettability.The modifier generation desorption not yet reacted of powder material 3 adsorptions that the agent that is modified after concussion is modified, the powder material 9 that the agent that is modified after the modifier that obtains not adsorbing on the removal surface is modified, powder material 5 surfaces that the agent that is not modified is modified, by water-wet, obtain the powder material 10 of being modified by the agent that is not modified of water-wet simultaneously.Then to annex solution paraffin body in container, can form the compound three-phase froth system of whiteruss, modified powder material and air in oscillatory process, removing the surface powder material 9 that agent that is modified after the modifier of absorption is not modified is easy to be adsorbed on the gas/liquid interface of the surface of the whiteruss emulsion droplets 12 in compound three-phase froth system or air/liquid paraffin bubble 12, and with water, separate in standing process, enter oil phase 2, be the whiteruss phase, and the powder material 10 of being modified by the agent that is not modified of water-wet enter water 4.
Below in conjunction with embodiment, the method for mensuration modified powder material degree of surface activation provided by the invention is described in further detail.
Industrial paper mill sludge after modification in embodiment 1-4 is by the modifier stearic acid, (to analyze pure respectively, Tianjin Yong Sheng Fine Chemical Co., Ltd), titanate esters NDZ311(technical grade, Nanjing dawn chemical industry company limited), Silane coupling agent KH550 (technical grade, Nanjing can Dehua work company limited) and odium stearate (analyze pure, Tianjin Yong Sheng Fine Chemical Co., Ltd) industrial paper mill sludge being carried out to modification obtains, the complicated component of industrial paper mill sludge wherein, comprise organism and inorganics, organism is mainly the cellulose of degrading in paper-making process, hemicellulose, lignin, inorganics is mainly filler (as calcium carbonate) and coating (as porcelain earth) and other inorganic salts that add in paper-making process.Concrete modification procedure is: take the wet industrial paper mill sludge (solid content is 35.25%) of preserving and be made into the suspending liquid that mass concentration is 8～12% under 5 ℃, suspending liquid is joined in there-necked flask, add thermal agitation, dropwise add the dilution of modifier under 80～90 ℃, wherein the addition of modifier is 1～5% of primary industry paper mill sludge over dry quality, filtration while hot after continuation stir process 60min, dry, grinding, cross the industrial paper mill sludge (its particle diameter≤250 μ m) after 60 mesh sieves obtain modification.
Embodiment 1:
1) will dry with the industrial paper mill sludge after stearic acid modified after 4h cooling 30min in silica gel drier under 105 ℃, to reach the over dry state, then take the industrial paper mill sludge (modified powder material) after the modification of 2.00g over dry, standby;
2) measuring 40mL distilled water joins in the 250mL pear shape separatory funnel, industrial paper mill sludge after the modification of the over dry that weighs up is joined to (solid-liquid ratio is 0.05g/mL) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 90 times, the powder material surface that the agent that makes in the modified powder material not to be modified is modified is by water-wet, then put down on filtration stand standing 30s gently;
3) measure the 40mL whiteruss and join (volume ratio of whiteruss and water is 1:1) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 120 times, the powder material that the agent that makes in the modified powder material to be modified is modified enters the oil phase consisted of whiteruss, the powder material that simultaneously makes surface be modified by the agent that is not modified of water-wet enters water, and standing 30min is to water and oil phase (whiteruss) layering;
4) by water and separation of oil, and the powder material modified of the disposable agent that is not modified that will enter in water puts in advance at the crucible type filtrator elimination moisture of 105 ℃ of lower constant weights, is placed in electric heating constant-temperature blowing drying box, under 105 ℃, is dried to constant weight;
5) calculate its activation index H=95% according to formula (1).
Embodiment 2:
1) will dry with the industrial paper mill sludge after titanate esters NDZ311 modification after 4h cooling 30min in silica gel drier under 100 ℃, to reach the over dry state, then take the industrial paper mill sludge (modified powder material) after the modification of 2.00g over dry, standby;
2) measuring 40mL distilled water joins in the 250mL pear shape separatory funnel, industrial paper mill sludge after the modification of the over dry that weighs up is joined to (solid-liquid ratio is 0.05g/mL) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 60 times, the powder material surface that the agent that makes in the modified powder material not to be modified is modified is by water-wet, then put down on filtration stand standing 30s gently.
3) measure the 40mL whiteruss and join (volume ratio of whiteruss and water is 1:1) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 150 times, the powder material that the agent that makes in the modified powder material to be modified is modified enters the oil phase consisted of whiteruss, the powder material that simultaneously makes surface be modified by the agent that is not modified of water-wet enters water, and standing 30min is to water and oil phase (whiteruss) layering;
4) by water and separation of oil, and the powder material modified of the disposable agent that is not modified that will enter in water puts in advance at the crucible type filtrator elimination moisture of 100 ℃ of lower constant weights, is placed in electric heating constant-temperature blowing drying box, under 100 ℃, is dried to constant weight;
5) calculate its activation index H=66% according to formula (1).
Embodiment 3:
1) will dry with the industrial paper mill sludge after the Silane coupling agent KH550 modification after 4h cooling 30min in silica gel drier under 110 ℃, to reach the over dry state, then take the industrial paper mill sludge (modified powder material) after the modification of 2.00g over dry, standby;
2) measuring 50mL distilled water joins in the 250mL pear shape separatory funnel, industrial paper mill sludge after the modification of the over dry that weighs up is joined to (solid-liquid ratio is 0.04g/mL) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 120 times, the powder material surface that the agent that makes in the modified powder material not to be modified is modified is by water-wet, then put down on filtration stand standing 30s gently.
3) measure the 25mL whiteruss and join (volume ratio of whiteruss and water is 1:2) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 90 times, the powder material that the agent that makes in the modified powder material to be modified is modified enters the oil phase consisted of whiteruss, the powder material that simultaneously makes surface be modified by the agent that is not modified of water-wet enters water, and standing 30min is to water and oil phase (whiteruss) layering;
4) by water and separation of oil, and the powder material modified of the disposable agent that is not modified that will enter in water puts in advance at the crucible type filtrator elimination moisture of 110 ℃ of lower constant weights, is placed in electric heating constant-temperature blowing drying box, under 110 ℃, is dried to constant weight;
5) calculate its activation index H=55% according to formula (1).
Embodiment 4:
1) will dry with the industrial paper mill sludge after the odium stearate modification after 4h cooling 30min in silica gel drier under 102 ℃, to reach the over dry state, then take the industrial paper mill sludge (modified powder material) after the modification of 2.00g over dry, standby;
2) measuring 100mL distilled water joins in the 500mL pear shape separatory funnel, industrial paper mill sludge after the modification of over dry joins (solid-liquid ratio is 0.02g/mL) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 80 times, the powder material surface that the agent that makes in the modified powder material not to be modified is modified is by water-wet, then put down on filtration stand standing 30s gently.
3) measure the 100mL whiteruss and join (volume ratio of whiteruss and water is 1:1) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 100 times, the powder material that the agent that makes in the modified powder material to be modified is modified enters the oil phase consisted of whiteruss, the powder material that simultaneously makes surface be modified by the agent that is not modified of water-wet enters water, and standing 30min is to water and oil phase (whiteruss) layering;
4) by water and separation of oil, and the powder material modified of the disposable agent that is not modified that will enter in water puts in advance at the crucible type filtrator elimination moisture of 102 ℃ of lower constant weights, is placed in electric heating constant-temperature blowing drying box, under 102 ℃, is dried to constant weight;
5) calculate its activation index H=83% according to formula (1).
The present invention is equally applicable to the purer inorganic particles of component such as calcium carbonate, silicon dioxide, titania are carried out the measurement of its modified product degree of surface activation after modification, and the embodiment 5 of below take describes as example.
Calcium carbonate after modification in embodiment 5 carries out modification by modifier stearic acid (analyzing pure, Tianjin Yong Sheng Fine Chemical Co., Ltd) to calcium carbonate and obtains, concrete modification procedure is: take 5g calcium carbonate in 45mL water, be made into the suspending liquid that mass concentration is 10%, suspending liquid is joined in there-necked flask, add thermal agitation, dropwise add the dilution of modifier under 80～90 ℃, wherein the addition of modifier is 3% of calcium carbonate quality, filtration while hot after continuation stir process 60min, dry, grinding, cross the calcium carbonate after 60 mesh sieves obtain modification.
Embodiment 5:
1) will dry with the calcium carbonate after stearic acid modified after 4h cooling 30min in silica gel drier under 108 ℃, to reach the over dry state, then take the calcium carbonate (modified powder material) after the modification of 2.00g over dry, standby;
2) measuring 40mL distilled water joins in the 250mL pear shape separatory funnel, calcium carbonate after the modification of the over dry that weighs up is joined to (solid-liquid ratio is 0.05g/mL) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 100 times, the powder material surface that the agent that makes in the modified powder material not to be modified is modified is by water-wet, then put down on filtration stand standing 30s gently;
3) measure the 10mL whiteruss and join (volume ratio of whiteruss and water is 1:4) in pear shape separatory funnel, after being built to lid, pear shape separatory funnel up and down reciprocatingly shakes 130 times, the powder material that the agent that makes in the modified powder material to be modified is modified enters the oil phase consisted of whiteruss, the powder material that simultaneously makes surface be modified by the agent that is not modified of water-wet enters water, and standing 30min is to water and oil phase (whiteruss) layering;
4) by water and separation of oil, and the powder material modified of the disposable agent that is not modified that will enter in water puts in advance at the crucible type filtrator elimination moisture of 108 ℃ of lower constant weights, is placed in electric heating constant-temperature blowing drying box, under 108 ℃, is dried to constant weight;
5) calculate its activation index H=99% according to formula (1).
Below the accuracy of the method for mensuration modified powder material degree of surface activation provided by the invention is carried out to experimental verification.
1. under identical reaction conditions, the effect of different modifying agents to industrial paper mill sludge modification:
The kind of modifier: 1# blank, 2# neopelex (chemical pure, the Solution on Chemical Reagents in Shanghai purchasing and supply station), the 3# stearic acid (is analyzed pure, Tianjin Yong Sheng Fine Chemical Co., Ltd), 4# maleic anhydride polyacrylate (MAPP, chemical pure, Honeywell company), 5# Silane coupling agent KH550 (technical grade, Nanjing energy Dehua work company limited), the 6# odium stearate (is analyzed pure, Tianjin Yong Sheng Fine Chemical Co., Ltd), 7# titanate esters NDZ311(technical grade, Nanjing dawn chemical industry company limited), 8# titanate esters NDZ401(technical grade, Nanjing dawn chemical industry company limited), 9# titanate esters NDZ311W(technical grade, Nanjing dawn chemical industry company limited).
A. adopt the single-phase measurement system of water to measure respectively the activation index of the industrial paper mill sludge after above-mentioned modifier modification (concrete modification operation is as embodiment 1), result is as shown in table 1.
Computing formula: the sample quality of activation index=float on the surface/sample gross mass * 100%
The activation index of the industrial paper mill sludge after the modification that the single-phase measurement system of table 1 employing water is measured
| Sequence number | Modifier | The single-phase measurement system of activation index/%(water) |
| 1# | Blank | 4.5 |
| 2# | Neopelex | 5.5 |
| 3# | Stearic acid | 5.5 |
| 4# | MAPP | 6 |
| 5# | KH550 | 6 |
| 6# | Odium stearate | 6.5 |
| 7# | NDZ311 | 7.5 |
| 8# | NDZ401 | 4.5 |
| 9# | NDZ311W | 6 |
B. adopt water of the present invention-oily two-phase measurement system to measure respectively the activation index of the industrial paper mill sludge after above-mentioned modifier modification (concrete modification operation is as embodiment 1), result is as shown in table 2, and wherein the volume ratio of whiteruss and water is 1:1.
Computing formula: the sample quality in activation index=oil phase/sample gross mass * 100%
Table 2 adopts the activation index of the industrial paper mill sludge after the modification that water-oily two-phase measurement system is measured
Qualitative checking method: get the tool plug graduated cylinder of 9 25mL, take each 2.00g of various modified products (over dry) and be added in the graduated cylinder of having numbered, to adding distil water in graduated cylinder to 20mL, standing observation.The water resisting property of finding 1#, 2# is the poorest, and just having added anhydrates soaks immediately; The water resisting property of 3#, 6# is best, crosses its surface of 3min and still is dry state; Remaining crosses 1min basically has wettingly, and the range estimation difference is not too large.Hence one can see that, the modified product that different modifier obtains under identical modified condition, and its water resisting property has notable difference.But the single-phase quantitative detecting analysis data of carrying out of water do not have discrimination, and regular very poor, and drawn data can not be corresponding to the viewed phenomenon of experiment.
And the data that water provided by the invention-oily two-phase measurement system draws have good discrimination.At first, each sample carries out 2 horizontal surveies, finds that the repeatability of data is better, can reflect the effect of modification.Secondly, the data trend quantitatively drawn and the experimental phenomena of observing coincide.So water provided by the invention-oily two-phase measurement system can be used as the quantitative measurment means of estimating the powder material activation degree.
2. the volume ratio of different liquids paraffin and water is measured the same modified product
Below under the measurement system of the volume ratio of different liquids paraffin and water, measure the same modification material best reagent of modified effect that above experiment draws---its activation index after the stearic acid modified industrial paper mill sludge of 3# (concrete modification operation is as embodiment 1), result is as shown in table 3.
The activation index of measuring under the volume ratio of table 3 different liquids paraffin and water
| Sequence number | The volume ratio of whiteruss and water | Activation index/% |
| 1# | 1:19 | 13 |
| 2# | 1:9 | 23 |
| 3# | 1:4 | 87 |
| 4# | 1:2.33 | 93 |
| 5# | 1:1.5 | 95 |
| 6# | 1:1 | 96 |
As shown in Table 3, different whiterusss and the volume ratio of water are larger on the impact of measurement result.When the volume ratio of whiteruss and water is 1:(9～19) time, the modified powder material still enters water mostly; When the volume ratio of whiteruss and water is 1:(1～4) time, resulting activation index is more stable, and the variation range of activation index is 87% to 96%, changes less.So this measurement system is when estimating the activation index of modified powder material, when the volume ratio of whiteruss and water is 1:(1～4) time better, especially the volume ratio when whiteruss and water is 1:(1～2.33) time best.
3. infrared analysis
This experiment is only chosen the different industrial paper mill sludge of stearic acid modified several activation indexs and has been carried out the FI-IR detection.As can be seen from Figure 3, stearic characteristic absorption peak appears at 2918cm
-1, 2850cm
-1and 1700cm
-1place is respectively-CH
3,-CH
2-and-the stretching vibration absorption peak of COOH.As shown in Figure 4, with blank mud powder (unmodified industrial paper mill sludge), a compares, and the mud powder c that the mud powder b that activation index is 56% after stearic acid modified and activation index are 100% after stearic acid modified is at 2921cm
-1, 2855cm
-1obvious absorption peak has appearred in place, and activation index is higher, the intensity at peak is larger, its activation index that water-oily two-phase measurement system draws is respectively 56% and 100%, from infrared analysis, what the surface coated stearic amount of mud powder after low stearic acid modified of activation index was 100% than the activation index really is few.
4. thermogravimetric analysis
The protection gas of thermogravimetric analysis experiment is nitrogen, and heating rate is 20 ℃/min.
Thermogravimetric analysis has been got 3 samples and has been respectively: the blank mud powder of 1#; The 2# activation index be 56% stearic acid modified after the mud powder; The 3# activation index be 100% stearic acid modified after the mud powder.
By Fig. 5-Fig. 7 can find out before modification and modification after its pyrolytic process of mud powder can be divided into roughly 4 stages: 1. moisture precipitation phase, temperature is approximately 30～150 ℃; 2. organic substance precipitation phase, temperature is approximately 150～600 ℃; 3. the catabolic phase of mineral matter, temperature is approximately 600～700 ℃; 4. in the residual stage of ash content, temperature is more than 700 ℃, and now the quality of mud powder pyrolysis residue remains unchanged substantially.
Can find out: in 350～600 ℃ of scopes, blank mud powder from there is different activation indexs stearic acid modified after modification after the mud powder between obvious difference is arranged.In order further illustrating, the TG curve of three kinds of samples to be processed and obtained table 4 by the TG analysis software.As can be seen from Table 4, between 30～150 ℃, the amount of the moisture that three samples are separated out is: 1# > 2# > 3#, this is the amount difference of getting due to each sample, and the amount of getting is more, and the quality of the moisture of separating out is just more; In addition, the initial water content of three kinds of samples is also influential to the mass loss rate of the moisture of separating out in the TG analytic process, and the initial aqueous rate is higher, and the mass loss rate of this stage moisture is just larger.The organic substance precipitation phase can be divided into two temperature sections, 150～350 ℃ of sections and 350～600 ℃ of sections.The mass loss rate of three samples of 150～350 ℃ of sections is: 1#<2#<3#, burning the mistake quality is: 3# > 1# > 2#, in this stage mud powder, contained organic fiber decomposes in a large number, lose quality by mass loss rate and burning and can infer to also have the part organic acid substance in this stage, comprise stearic acid generation pyrolysis, the activation index of 3# sample is 100%, surface coated stearic acid is more, although the sample size that causes 3# to get is minimum, maximum in the loss on ignition of this stage 3# sample.The mass loss rate of three samples of 350～600 ℃ of sections is: 1#<2#<3#, and burning is lost quality and is: 1#<2#<3#, and differ greatly each other, infer thus in this stage a large amount of stearic acid generation pyrolysis is arranged.In conjunction with stearic physical property: boiling point is: 232 ℃, decomposition temperature are 376 ℃, are 444.3 ℃ naturally, in addition, calcium carbonate or the porcelain earth on stearic acid and mud powder surface can react, produce chemical bond, so pyrolysis will, higher than pure stearic acid, mainly occur in its pyrolysis temperature of stearic acid that Sludge Surface coats between 350～600 ℃.Getting the data of 350～600 ℃ of sections is analyzed:
The mass loss rate of the blank mud powder of 1# is: W
1=7.816%
The mass loss rate of the mud powder after 2# activation index 56% stearic acid modified is: W
2=8.612%
The mass loss rate of the mud powder after 3# activation index 100% stearic acid modified is: W
3=10.129%
So estimation can draw:
The stearic acid covering amount of the mud powder after the 2# modification is about W
2-W
1=0.796%
The stearic acid covering amount of the mud powder after the 3# modification is about W
3-W
1=2.313%
The pyrolysis data of the mud powder after the modification that the blank mud powder of table 4 and activation index are 56% and 100%
In sum, the coating degree that the method for mensuration modified powder material degree of surface activation provided by the present invention can reaction modifying powder material surface modifier.Activation index is higher, and the amount of the surface coated modifier of modified powder material is just more, and the modification degree is more complete.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading instructions of the present invention, be claim of the present invention and contain.
Claims (10)
1. a method of measuring modified powder material degree of surface activation is characterized in that:
1) first water is joined in container, then the modified powder material of over dry is joined in container, wherein the modified powder material is that powder material by surface hydrophilicity is modified after the agent modification and obtains, the solid-liquid ratio of modified powder material and water is 0.02～0.05g/mL, by seal of vessel concussion, the powder material surface that the agent that makes in the modified powder material not to be modified is modified is by water-wet, then standing;
2) add whiteruss again in container, then by seal of vessel concussion, the powder material that the agent that makes in the modified powder material to be modified is modified enters the oil phase consisted of whiteruss, the powder material that simultaneously makes surface be modified by the agent that is not modified of water-wet enters water, more standing water and oil phase layering to container; The volume ratio of the water added in the whiteruss wherein added and step 1) is 1:(1～4);
3) by water and separation of oil, and will enter the powder material that the agent that is not modified in water modifies and be dried to constant weight;
4) press the activation index H that formula (1) calculates the modified powder material:
Wherein: m
1the dried quality of powder material for the agent modification that is not modified in step 3); The quality that m is the modified powder material that adds in step 1).
2. the method for mensuration modified powder material degree of surface activation according to claim 1, is characterized in that: the powder that the powder material in described step 1) is calcium carbonate, silicon dioxide, titania or industrial sludge formation.
3. the method for mensuration modified powder material degree of surface activation according to claim 1 and 2, it is characterized in that: the modifier in described step 1) is neopelex, stearic acid, maleic anhydride polyacrylate, Silane coupling agent KH550, odium stearate, titanate esters NDZ311, titanate esters NDZ401 or titanate esters NDZ311W.
4. the method for mensuration modified powder material degree of surface activation according to claim 3, it is characterized in that: the be modified concrete steps of agent modification of described powder material are: powder material is made into to the suspending liquid that mass concentration is 8～12%, add thermal agitation, dropwise add the dilution of modifier under 80～90 ℃, wherein the quality of modifier is 1～5% of powder material quality, filtration while hot after continuation stir process 60min, dry, grinding, sieve and obtain the modified powder material.
5. the method for mensuration modified powder material degree of surface activation according to claim 1 and 2, it is characterized in that: the particle diameter of described modified powder material is 1nm～250 μ m.
6. the method for mensuration modified powder material degree of surface activation according to claim 1 and 2, it is characterized in that: the modified powder material of the over dry in described step 1) obtains after cooling 30min after the modified powder material is dried to 4h under 100～110 ℃ in silica gel drier.
7. the method for mensuration modified powder material degree of surface activation according to claim 1 and 2, it is characterized in that: the concussion in described step 1) is for up and down reciprocatingly shaking 60～120 times; Time of repose is 30s.
8. the method for mensuration modified powder material degree of surface activation according to claim 1 and 2, it is characterized in that: described whiteruss is chemical pure, its principal ingredient is C
16～C
20n-alkane, density is 0.86～0.905.
9. the method for mensuration modified powder material degree of surface activation according to claim 1 and 2, it is characterized in that: the concussion described step 2) is for up and down reciprocatingly shaking 90～150 times; Time of repose is 30min.
10. the method for mensuration modified powder material degree of surface activation according to claim 1 and 2, it is characterized in that: the concrete operations that the powder material that the agent that will not be modified in described step 3) is modified is dried to constant weight are that powder material that the agent that is not modified in water is modified is first put in advance the crucible type filtrator elimination moisture 100～110 ℃ of lower constant weights, be placed in again electric heating constant-temperature blowing drying box, under 100～110 ℃, be dried to constant weight.
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| CN112108073A (en) * | 2019-06-21 | 2020-12-22 | 南京泰佳化工有限公司 | Crystal 80 type powdery sodium alkyl benzene sulfonate |
| CN113063702A (en) * | 2021-03-29 | 2021-07-02 | 中国石油大学(华东) | Novel evaluation method suitable for formation silt solid particle surface wettability |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107976512A (en) * | 2016-12-14 | 2018-05-01 | 广西强荣实业有限公司 | A kind of inorganic particle aqueous sample activation rate test device and method |
| CN107271313A (en) * | 2017-07-24 | 2017-10-20 | 深圳大学 | A kind of method of testing of inorganic phase-changing material modified effect |
| CN107271313B (en) * | 2017-07-24 | 2019-03-19 | 深圳大学 | A kind of test method of inorganic phase-changing material modified effect |
| CN108931419A (en) * | 2018-07-18 | 2018-12-04 | 广西贺州市科隆粉体有限公司 | A kind of detection method of calcium carbonate powder activation grade |
| CN108931419B (en) * | 2018-07-18 | 2021-03-23 | 广西贺州市科隆粉体有限公司 | Method for detecting activation degree of calcium carbonate powder |
| CN112108073A (en) * | 2019-06-21 | 2020-12-22 | 南京泰佳化工有限公司 | Crystal 80 type powdery sodium alkyl benzene sulfonate |
| CN113063702A (en) * | 2021-03-29 | 2021-07-02 | 中国石油大学(华东) | Novel evaluation method suitable for formation silt solid particle surface wettability |
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