CN102636406B - Method for measuring water absorbing capacity of silica - Google Patents
Method for measuring water absorbing capacity of silica Download PDFInfo
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- CN102636406B CN102636406B CN 201210131883 CN201210131883A CN102636406B CN 102636406 B CN102636406 B CN 102636406B CN 201210131883 CN201210131883 CN 201210131883 CN 201210131883 A CN201210131883 A CN 201210131883A CN 102636406 B CN102636406 B CN 102636406B
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Abstract
The invention discloses a method for measuring water absorbing capacity of silica. The method comprises the following steps of: (1), weighing silica with a certain weight, and dispersing the silica into distilled water to ensure that the mass ratio of the silica to the distilled water is 1: (5-10) to obtain a water dispersion solution of the silica; (2), adding the water dispersion solution of the silica into a solvent filter, filtering under the vacuum degree of (-0.98)-(-0.92)MPa until no water drops are pumped out, and keeping the vacuum degree for 10min to obtain a filter cake after the silica absorbs water; (3), measuring the water content Q of the filter cake of the silica on a water measurer; and (4), obtaining the water absorbing capacity W from the measured water content Q according to a formula of W=Q*100/K, wherein K represents an experience correlation coefficient of the water content Q and the water absorbing capacity W.
Description
Technical field
The present invention relates to a kind of assay method of silicon dioxide water absorbing capacity, especially relate to the assay method that a kind of toothpaste is used the silicon dioxide water absorbing capacity.
Background technology
Toothpaste is a kind of water wettability system that is evenly mixed by various ingredients.The silicon dioxide that is applied in the toothpaste is called toothpaste silicon dioxide, have good thixotropy and friction spatter property, and chemical property is stable, not with toothpaste in other composition (as fluoride, Chinese herbal medicine, spices etc.) react, have best compatibility.
The water absorptivity of silicon dioxide and water absorbing capacity thereof produce significant effects to usability, the stability of toothpaste.Water absorbing capacity is toothpaste with the important performance indexes of silicon dioxide, accurately controls and measures toothpaste and have great importance to producing toothpaste and controlling silicon dioxide character with the water absorbing capacity of silicon dioxide.The silicon dioxide that adds in the toothpaste can be divided three classes i.e. friction type, comprehensive, thickening type by the usability branch at present.The toothpaste industry generally defines with the more satisfactory quality of silicon dioxide three class toothpaste by water absorbing capacity and is at present: the water absorbing capacity scope of every 20g friction type silicon dioxide is 16ml ~ 19ml, every 20g is comprehensive for the water absorbing capacity scope of silicon dioxide is 30ml ~ 33ml, and the water absorbing capacity scope of every 20g thickening type silicon dioxide is 43ml ~ 45ml.Thereby determine that by the water absorbing capacity of measuring silicon dioxide it belongs to any type, thereby determine its different application in tooth paste product.
Measurement toothpaste is to adopt the assay method of water absorbing capacity among the QB/T 2346-2007 " toothpaste silicon dioxide " with the water absorbing capacity of silicon dioxide at present, this method adopts the buret titrimetry, its key step is: take by weighing sample 20g (being accurate to 0.01g) and place dry enamelled cup, gradually splash into distilled water 2mL～3mL from buret, make sample powder uniform water absorption, constantly stir with spatula, constantly splash into and shake, all become a ball not loose until the sample powder and be terminal point, show water absorbing capacity with the milliliter numerical table that consumes distilled water, unit is ml.This method of testing complex steps, manual operation error are very big, and its error range is greater than ± 2, are very easy to cause toothpaste with the affiliated type misjudgment of silicon dioxide, finally cause using makeing mistakes even producing underproof tooth paste product.
Summary of the invention
In view of the above, be necessary to provide a kind of assay method of easy and simple to handle, efficient is high, personal error is less silicon dioxide water absorbing capacity.
A kind of assay method of silicon dioxide water absorbing capacity comprises the steps:
(1) takes by weighing the silicon dioxide of constant weight, it is dispersed in the distilled water, obtain the aqueous dispersions of silicon dioxide; Preferably, the mass ratio of silicon dioxide and distilled water is 1:5～10, can obtain the water dispersion pulp liquid of uniform silicon dioxide.
(2) aqueous dispersions with silicon dioxide is added in the filtrator, carries out suction filtration under certain vacuum tightness, makes the silicon dioxide suction filter cake after saturated; Preferably, be-0.98 in vacuum tightness～-0.92MPa air pressure under suction filtration, till no longer including water droplet and extracting out, and under this vacuum tightness, keep 5-15min, obtain the filter cake of silicon dioxide suction after saturated.
(3) silica filter cake is measured water percentage Q in its filter cake by moisture teller; Wherein, it is DENVER(U.S. Denver that moisture teller can adopt marque) moisture teller of IR-35, the moisture teller that also can adopt the black minute any family of instrument company in Weifang Zhong Te Electron equipment Co., Ltd, Shanghai flood discipline instrument and equipment company limited or Zibo to produce
(4) by experimental formula W=Q of the present invention * 100/K, obtain water absorbing capacity W value, its error range is less than ± 0.5, wherein the experience related coefficient K value corresponding with water percentage Q in above-mentioned experimental formula and the experimental formula, obtain via test of many times, derivation can be joined aftermentioned embodiment.So, can roughly determine the toothpaste type of silicon dioxide by described water percentage Q, and corresponding experience related coefficient K, type is as follows:
(1) silica filter cake water percentage Q between 50%～60% for the friction type, experience related coefficient K is about 3.15, the water absorbing capacity W of corresponding friction type silicon dioxide be 16ml ~ 19ml;
(2) silica filter cake water percentage Q is comprehensive between 67%～74%, and experience related coefficient K is about 2.25; The water absorbing capacity of corresponding comprehensive silicon dioxide be 30ml ~ 33ml;
(3) silica filter cake water percentage Q is thickening type between 80%～83%, and experience related coefficient K is about 1.85; The water absorbing capacity of corresponding thickening type silicon dioxide be 43ml ~ 45ml.
Compared to prior art, the present invention measure toothpaste with the assay method of silicon dioxide water absorbing capacity by silicon dioxide to be measured is scattered in water earlier, the suction suction filtration forms filter cake, then by the water percentage Q in the moisture teller mensuration filter cake, draw the type of silicon dioxide, draw in then according to the present invention the empirical parameter K of corresponding silicon dioxide type, by experimental formula W=Q * 100/K, namely can be regarded as the water absorbing capacity of corresponding silicon dioxide.More traditional method of passing through the silicon dioxide water absorbing capacity that the buret titrimetry records, method of the present invention is more accurate, and easy and simple to handle, efficient is high, personal error is less.
Embodiment
Be described further below in conjunction with the present invention of embodiment.
The derivation of the experience related coefficient K corresponding with water percentage Q please be joined following embodiment 1,2 in above-mentioned experimental formula W=Q * 100/K and the experimental formula:
Embodiment 1
Take by weighing 20g silicon dioxide, it is dispersed in the 200g distilled water, obtain the aqueous dispersions of uniform silicon dioxide; (2) aqueous dispersions with silicon dioxide is added in the filtrator, carries out suction filtration under the vacuum tightness of-0.93MPa, till no longer including water droplet and extracting out, keeps vacuum tightness 10min, obtains the filter cake of silicon dioxide suction after saturated; (3) the water percentage Q that silica filter cake is measured in its filter cake at moisture teller is 69.2%.
Take by weighing the 20g silicon dioxide of identical weight, assay method according to water absorbing capacity among the QB/T 2346-2007 " toothpaste silicon dioxide " adopts the buret titrimetry, distilled water in the buret is splashed in the dry enamelled cup that the silicon dioxide sample is housed, constantly stir, constantly splash into and shake, become entirely until the sample powder and stop when a ball does not loose.The water absorbing capacity W that records this silicon dioxide by this buret titrimetry is 30.2ml.Get the 20g silicon dioxide of identical weight, the buret titrimetry repeats repeatedly like this, as repeats 10 times, and can obtain water-intake rate W respectively is 30.2ml, 30.8ml, 31.8 ml, 30.3 ml, 31.1 ml, 30.5 ml, 31.5 ml, 30.7 ml, 30.5 ml, 30.6 ml.According to the water absorbing capacity of measuring as can be known, the type of silicon dioxide belongs to comprehensive.If Q and W are analyzed in coordinate diagram, can find out that Q and W have certain linear, if K=Q * 100/W, then K is respectively 2.29,2.25,2.18,2.28,2.23,2.27,2.20,2.25,2.27,2.26, K and averages and be about 2.25.
Embodiment 2
Take by weighing 20g silicon dioxide, it is dispersed in the 100g distilled water, obtain the aqueous dispersions of uniform silicon dioxide; (2) aqueous dispersions with silicon dioxide is added in the filtrator, carries out suction filtration under the vacuum tightness of-0.98MPa, till no longer including water droplet and extracting out, keeps vacuum tightness 15min, obtains the filter cake after the silicon dioxide suction; (3) the water percentage Q that silica filter cake is measured in its filter cake at moisture teller is 72.50%.
Take by weighing the 20g silicon dioxide of identical weight, assay method according to water absorbing capacity among the QB/T 2346-2007 " toothpaste silicon dioxide " adopts the buret titrimetry, distilled water in the buret is splashed in the dry enamelled cup that the silicon dioxide sample is housed, constantly stir, constantly splash into and shake, become entirely until the sample powder and stop when a ball does not loose.The water absorbing capacity W that records this silicon dioxide by this buret titrimetry is 32.6ml.Get the 20g silicon dioxide of identical weight, the buret titrimetry repeats repeatedly like this, as, repeat 10 times, can obtain water-intake rate W respectively is 32.6 ml, 32.1 ml, 31.9 ml, 32.7 ml, 30.9ml, 32.5 ml, 32.4 ml, 32.9 ml, 31.1 ml, 32.8 ml.According to water-intake rate as can be known, the type of silicon dioxide is comprehensive.W and Q are analyzed in coordinate diagram, can find out that Q and W still have certain linear, if K=Q * 100/W, then K is respectively 2.22,2.26,2.27,2.21,2.34,2.23,2.23,2.20,2.33,2.21, K and averages and be about 2.25.
Can find out that from embodiment 1 and embodiment 2 the water percentage Q in filter cake is 69.2% or at 72.5% o'clock, K averages and is 2.25.In order to prove this experience factor K value, can work as the Q value not simultaneously further further combined with more test data, equally can be according to above-mentioned experimental technique, the comparatively ideal water absorbing capacity 30ml of comprehensive silicon dioxide ~ 33ml scope in, by experiment many times, obtain the K value and be about 2.25.
Equally according to said method, by test and test many times, when silica filter cake water percentage Q 50%～60%, the experience related coefficient K value of its water percentage Q and water absorbing capacity W is about 3.15, this moment, the water absorbing capacity scope of silicon dioxide was 16ml ~ 19ml, belonged to the friction type; When silica filter cake water percentage Q 80%～83%, the experience related coefficient K value of its water percentage Q and water absorbing capacity W is about 1.85, this moment silicon dioxide the suction scope be 43ml ~ 45ml, belong to thickening type.
And by verification experimental verification, the water absorbing capacity of the silicon dioxide that obtains according to above-mentioned experimental formula W=Q * 100/K, the water absorbing capacity of the silicon dioxide that records than traditional manual titrimetry is more accurate, can reduce the personal error that manual titrimetry causes.
According to push away experimental formula W=Q * 100/K and experimental formula in the experience related coefficient K corresponding with water percentage Q, be applied among the following embodiment 3-5 to draw the water absorbing capacity of silicon dioxide.
Embodiment 3
(1) takes by weighing silica 1 5g, it is dispersed in the 120g distilled water, obtain the aqueous dispersions of silicon dioxide;
(2) aqueous dispersions with silicon dioxide is added in the solvent filter, carries out suction filtration under the vacuum tightness of-0.93MPa, till no longer including water droplet and extracting out, keeps vacuum tightness 10min, obtains the filter cake after the silicon dioxide suction;
(3) the water percentage Q that silica filter cake is measured in its filter cake at moisture teller is 58.66%;
(4) be 58.66% according to water percentage Q, the type of determining this silicon dioxide is the friction type, and the experience related coefficient K of its water percentage Q and water absorbing capacity W can be taken as 3.15;
(5) according to water absorbing capacity W=Q * 100/K, calculating water absorbing capacity is 18.6 ml.
Embodiment 4
(1) takes by weighing silica 1 0g, it is dispersed in the 100g distilled water, obtain the aqueous dispersions of silicon dioxide;
(2) aqueous dispersions with silicon dioxide is added in the solvent filter, carries out suction filtration under the vacuum tightness of-0.95MPa, till no longer including water droplet and extracting out, keeps vacuum tightness 10min, obtains the filter cake after the silicon dioxide suction;
(3) the water percentage Q that silica filter cake is measured in its filter cake at moisture teller is 70.75%;
(4) be 70.75% according to water percentage Q, the type of determining this silicon dioxide is comprehensive, and the experience related coefficient K of its water percentage Q and water absorbing capacity W can be taken as 2.25;
(5) according to water absorbing capacity W=Q * 100/K, calculating water absorbing capacity is 31.4 ml.
Embodiment 5
(1) takes by weighing toothpaste silicon dioxide 25g, it is dispersed in the 150g distilled water, to the aqueous dispersions of silicon dioxide;
(2) aqueous dispersions with silicon dioxide is added in the solvent filter, carries out suction filtration under the vacuum tightness of-0.97MPa, till no longer including water droplet and extracting out, keeps vacuum tightness 10min, obtains the filter cake after the silicon dioxide suction;
(3) the water percentage Q that silica filter cake is measured in its filter cake at moisture teller is 80.18%;
(4) be 80.18% according to water percentage Q, the type of determining this silicon dioxide is thickening type, and the experience related coefficient K of its water percentage Q and water absorbing capacity W can be taken as 1.85;
(5) according to water absorbing capacity W=Q * 100/K, calculating water absorbing capacity is 43.3 ml.
For comparison test result's accuracy, adopt repeatedly the method for manual titration to draw the suction value to above-described embodiment 3 ~ 5.
Embodiment 3 adopts the method for manual titration, takes by weighing the 10g silicon dioxide of identical weight, according to the assay method employing buret titrimetry of water absorbing capacity among the QB/T 2346-2007 " toothpaste silicon dioxide ", repeat 10 times, can obtain water-intake rate W respectively is 18.2ml, 18.4ml, 18.1ml, 18.4 ml, 18.6 ml, 18.6 ml, 18.7ml, 18.1ml, 17.7 ml, 17.9 ml.
As seen, the concentrated scope of manual repeatedly titration is between 18.2-18.7, and silicon dioxide water absorbing capacity 18.6 ml that the method for the invention records, and value of the present invention is more accurate, and personal error is less, and easy and simple to handle, efficient is high.
Embodiment 4 adopts the method for manual titration, takes by weighing the 15g silicon dioxide of identical weight, according to the assay method employing buret titrimetry of water absorbing capacity among the QB/T 2346-2007 " toothpaste silicon dioxide ", repeat 10 times, can obtain water-intake rate W respectively is 31.3 ml, 31.6 ml, 30.2 ml, 31.4 ml, 31.7 ml, 31.8 ml, 32.3ml, 31.9ml, 32.7 ml, 32.4 ml.
As seen, the concentrated scope of manual repeatedly titration is between 31.3-31.9, and silicon dioxide water absorbing capacity 31.4 ml that the method for the invention records, and value of the present invention is more accurate, and personal error is less, and easy and simple to handle, efficient is high.
Embodiment 5 adopts the method for manual titration, takes by weighing the 25g silicon dioxide of identical weight, according to the assay method employing buret titrimetry of water absorbing capacity among the QB/T 2346-2007 " toothpaste silicon dioxide ", repeat 10 times, can obtain water-intake rate W respectively is 42.1 ml, 43.6 ml, 43.2 ml, 41.4 ml, 43.3 ml, 43.5 ml, 41.8ml, 43.4ml, 43.2 ml, 40.7ml.
As seen, the concentrated scope of manual repeatedly titration is between 43.2-43.5, and silicon dioxide water absorbing capacity 43.3 ml that the method for the invention records, and value of the present invention is more accurate, and personal error is less, and easy and simple to handle, efficient is high.
To sum up, the present invention measures toothpaste and uses the assay method of silicon dioxide water absorbing capacity by earlier silicon dioxide to be measured being disperseed suction formation filter cake, measure water percentage in its filter cake by moisture teller then, the experimental formula W=Q that draws in then according to the present invention * 100/K and empirical parameter K, namely can be regarded as the water absorbing capacity of silicon dioxide, draw the type of silicon dioxide.More traditional method of passing through the silicon dioxide water absorbing capacity that the buret titrimetry records, method of the present invention is more accurate, and easy and simple to handle, efficient is high, personal error is less.
The above only is the preferred embodiments of the present invention; be not so limit claim of the present invention; every equivalent transformation that utilizes description of the present invention to do, or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (9)
1. the assay method of a silicon dioxide water absorbing capacity comprises the following steps:
Take by weighing the silicon dioxide of constant weight, it is dispersed in the distilled water, obtain the aqueous dispersions of silicon dioxide;
The aqueous dispersions of silicon dioxide is added in the solvent filter, under vacuum tightness, carries out suction filtration, make the filter cake after silicon dioxide absorbs water;
It is characterized in that:
Filter cake is measured water percentage Q in its filter cake by moisture teller;
By experimental formula W=Q * 100/K, obtain water absorbing capacity W value;
Wherein, the experience related coefficient K of the water percentage Q of described water percentage Q value correspondence is as follows: water percentage Q is 50%～60%, and experience related coefficient K is 3.15; Q is 67%～74%, and experience related coefficient K is 2.25; Water percentage Q is 80%～83%, and experience related coefficient K is 1.85.
2. the assay method of silicon dioxide water absorbing capacity according to claim 1 is characterized in that: described water percentage Q value is between 50%～60% the time, and the water absorbing capacity scope of silicon dioxide is 16ml～19ml, belongs to the friction type.
3. the assay method of silicon dioxide water absorbing capacity according to claim 1 is characterized in that: described water percentage Q value is between 67%～74% the time, and the water absorbing capacity scope of silicon dioxide is 30ml～33ml, belongs to comprehensive.
4. the assay method of silicon dioxide water absorbing capacity according to claim 1 is characterized in that: described water percentage Q value is between 80%～83% the time, and the water absorbing capacity scope of silicon dioxide is 43ml～45ml, belongs to thickening type.
5. the assay method of silicon dioxide water absorbing capacity according to claim 1, it is characterized in that: described silicon dioxide is dispersed in the distilled water, and the mass ratio of silicon dioxide and distilled water is 1:5～10.
6. the assay method of silicon dioxide water absorbing capacity according to claim 1 is characterized in that: when the aqueous dispersions of described silicon dioxide carried out suction filtration under vacuum tightness, vacuum tightness was-0.98～-0.92MPa.
7. the assay method of silicon dioxide water absorbing capacity according to claim 6 is characterized in that: described suction filtration to filter cake no longer includes water droplet extract out till, and under vacuum tightness, keep taking out behind the 5-15min.
8. the assay method of silicon dioxide water absorbing capacity according to claim 1 is characterized in that: it is the moisture teller of DENVER IR-35 that described moisture teller adopts marque.
According to as claim 1-8 any one the assay method of silicon dioxide water absorbing capacity, it is characterized in that: be applied to measure toothpaste with the water absorbing capacity of silicon dioxide.
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| CN111426592A (en) * | 2020-04-08 | 2020-07-17 | 攀钢集团重庆钒钛科技有限公司 | Method for detecting water absorption capacity of titanium dioxide |
| CN114199712A (en) * | 2021-11-26 | 2022-03-18 | 金三江(肇庆)硅材料股份有限公司 | Method for measuring oil absorption value of silicon dioxide |
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