CN102323194A - Detection method for particle size of polymer polyol - Google Patents
Detection method for particle size of polymer polyol Download PDFInfo
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- CN102323194A CN102323194A CN201110243818A CN201110243818A CN102323194A CN 102323194 A CN102323194 A CN 102323194A CN 201110243818 A CN201110243818 A CN 201110243818A CN 201110243818 A CN201110243818 A CN 201110243818A CN 102323194 A CN102323194 A CN 102323194A
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- polymer polyatomic
- detection method
- granularity
- polyatomic alcohol
- polymer polyol
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Abstract
The present invention relates to a detection method for a particle size of a polymer polyol. In the prior art, the detection method is not applicable for the polymer polyol, or the error of the detection result is big. To solve the technical problems in the prior art, the present invention provides the detection method for the particle size of the polymer polyol. The method comprises the following process steps: weighing a polymer polyol sample; diluting the sample through a solvent; filtering through a screen; placing the filtered particles and the screen in a vacuum drier to carry out drying; cooling the filtered particles and the screen to a room temperature after completing drying, then weighing and calculating the particle size of the sample. The method provided by the present invention is a physical separation method; with the method, the loss of the active ingredients of the polymer polyol during the separation process can be effectively prevented, the active ingredients of the polymer polyol can be maximally preserved, the particles in the polymer polyol can be effectively separated from the sample through the physical separation, the elementary substances and a certain amount of the compounds can be removed, the detected particle size of the polymer polyol is accurate, and the precision of the detected particle size is high.
Description
Technical field
The present invention relates to a kind of detection method of polymer polyatomic alcohol granularity.
Background technology
The graft polymer polyvalent alcohol is the polymer polyatomic alcohol with certain particle size, and polymer polyatomic alcohol is to form graft polymer by polymerization of mixtures such as conventional polyether glycol and the basic polyethers of part and vinyl monomer, initiating agent, chain-transferring agents.Polymer polyatomic alcohol is claimed white polyether polymer polyvalent alcohol again, is used to prepare the soft and semi-hard polyurethane foam plastic goods of high-mechanic or high-modulus.Polymer polyatomic alcohol (POP) is widely used in making high resilience, high-mechanic, the soft foam of high rigidity PU.
The polymerized polyalcohol product quality has determined its application and with the performance of its polyurethane that makes.Adopt or all adopt this organic filling polyethers to replace general polyether glycol in foaming industry part, but production density is low and polyfoam that load-carrying properties are high had both reached hardness requirement, conservation again is so welcome by producer very.
Along with people's improves constantly the polyurethane product performance requirement, and the raising of isocyanurate foam performance is that granule size, what, the granularity of polymkeric substance of solid content, polymkeric substance with polymer polyatomic alcohol is that dispersive property and polymer morphology change.Polymer polyatomic alcohol is styrene and vinyl cyanide high concentration dispersion after the dispersin polymerization in the polyethers medium; Its main technical requirements is the dispersive property of high solid content (40%), low work viscosity (4000mPa.s～6000m Pa.s/25 ℃) and good stable property and dispersion, the performance of POP fine particlesization, homogenization degree.The quality of POP granularity is reflecting the effect of dispersive property, yield etc., for this reason, need find out the method for the scientific and reasonable test granularity of simple possible.Testing graininess is an experimental work that the split particle property is characterized through specific instrument and method.The application of powder in our daily life and industrial and agricultural production is very extensive, but detects just considerably less to high viscosity viscosity liquid.Requirement to granularity in different applications is to have nothing in common with each other, and in the index of all reflection particle properties, size-grade distribution is a very important job of greatest concern in the used application.
Following mask body is done related notion and is simply explained:
1, particle: in the certain size scope, have the solid of given shape, the certain size that here refers to generally at millimeter between the nanometer, particle not only refers to solid particle, also has liquid particles such as droplet, oil droplet.
2, powder: the particle swarm of forming by a large amount of particles of different sizes.
3, granularity: the size of particle is called the granularity of particle.
4, the distribution of granularity: the different-grain diameter particle that reflects with specific instrument and method accounts for the percentage of overall total amount; Be divided into interval the distribution and two kinds of forms of cumulative distribution again; The interval distribution is called differential again and distributes or frequency distribution, and it representes the percentage composition of particle in a series of particle size interval, and cumulative distribution claims that also score distributes, its expression less than or greater than the percentage composition of certain particle diameter particle.
5, equivalent grain size: particle diameter is exactly the diameter of particle.Have only spherosome that diameter is just arranged; Other shapes do not have a diameter, but various erose, have sheet, needle-like, many ribs shape or the like; These complicated particles are can not be directly to represent its size with this notion of diameter theoretically; And the diameter of granularity is size the most directly perceived of describing a particle in real work, when the simplest amount, equivalent grain size refer to that the spheric grain when a certain physical characteristics of a particle and homogeneity is identical or close; Just represent the diameter of this actual particle with the diameter of this spheric grain, the particle diameter of this spheric grain is exactly the equivalent grain size of this actual particle so.
At present viscosity of polyether can detect through viscosity meter effectively and accurately, and the detection of granularity is relative complex then, and the method for testing graininess is a lot, and commonly used at present have sedimentation, sieve method and an electric-resistivity method.Sedimentation is a kind of method according to the settling velocity different measuring size-grade distribution of particle in liquid of different-grain diameter; Its basic process is to be put into sample to process certain density suspending liquid in certain solution, and the particle in the suspending liquid under gravity or centrifugal action sedimentation will take place.Test process is at first quantity of sample and liquid to be mixed with suspending liquid in the 500ml graduated cylinder; Stir the back and take out a certain amount of (like 20ml) general assembly (TW) as sample; Calculate good every kind of Granula Subsidence Time according to the Stokes law again; Emit the suspending liquid of same amount respectively in the fixing moment, represent the particle diameter of this moment correspondence, calculate granularity.Sieve method is a kind of traditional testing graininess method, and it is to make particle test granularity through the sieve aperture of different size.Can control the percent of pass of particle diameter particle with sieve.Electric-resistivity method is Ku Ertefa again, is moment through a little micropore again according to particle, and the segment space that has occupied in the little micropore has arranged the conducting liquid in the little micropore, the principle test size-grade distribution that the resistance at little micropore two ends is changed.
There is following problem respectively in said method in practice: 1, polymer polyatomic alcohol is that a kind of high viscosity dope can regular generation sedimentation; And the polymer polyatomic alcohol outward appearance is generally white or the opaque liquid of shallow milk yellow; Can not remove the organic influence of some monomers; With the visual sedimentation that can't observe particle, sedimentation is inapplicable.2, normally electric conductivity is preferably for the employed medium of electric-resistivity method.The solvent electric conductivity that polymer polyatomic alcohol uses is relatively poor, and the resultant error that electric-resistivity method is measured is too big.3, traditional sieve method generally is to be used for measuring powder, and polymer polyatomic alcohol is a kind of high viscosity dope, and liquid is difficult to pass through fully filter screen, can stick on filter screen.Above-mentioned three kinds of methods problem that all existence can't be used or error is too big in measuring grafted polyether polyol can't meet the demands.So need the detection method that a kind of accuracy is high, precision is high.
Summary of the invention
Be not suitable for graft polymer polyvalent alcohol or the too big technical matters of testing result error for solving existing detection method, the present invention proposes a kind of method that quick and precisely detects graft polymer polyvalent alcohol granularity and distribution situation thereof.
Technical scheme of the present invention is: a kind of detection method of polymer polyatomic alcohol granularity; Processing step is following: take by weighing said polymer polyatomic alcohol sample; With passing through strainer filtering behind the solvent dilution; Place vacuum dryer to carry out drying together with filter screen the particle that leaches, weigh after after drying finishes the particle that leaches and filter screen being cooled to room temperature, calculate the granularity of sample.The method is called the screening filtration method.
Said filter screen is selected the stainless steel material filter screen for use, and its order number is 150 orders, and its size is preferably length * wide * height: 5cm * 5cm * 2cm.
Said solvent is selected a kind of in isopropyl alcohol, ethanol, acetone or the methyl alcohol for use.
The addition of said solvent is 100～300ml.
The amount of taking by weighing of said polymer polyatomic alcohol sample is 1～100g, and preferred 10～80g, optimum are 30～50g.
Said vacuum drying chamber temperature is controlled at 70～120 ℃, preferred 70～90 ℃.
Be 5～20 minutes said drying time, preferred 5～10 minutes.
Beneficial effect of the present invention is: the screening filtration method that the present invention adopts is a kind of Physical Separation Technology; In its detachment process, can prevent the polymer polyatomic alcohol loss of active ingredients effectively; Especially full-bodied sample is preserved the active component of polymer polyatomic alcohol to greatest extent.Can effectively the granularity in the polymer polyatomic alcohol (POP) be separated from sample with physical separation with this detection method; Remove simple substance and the compound under certain order number; Calculate the content of component to be measured in sample, record that the polymer polyatomic alcohol granularity is accurate, precision is high.This detection method is that polymer polyatomic alcohol provides favourable data, instructs technological parameter, technological operation, makes polymer polyatomic alcohol reach viscosity and granularity, solid content rationality have directive significance.
Embodiment
Below through embodiment the present invention is described.
Embodiment 1:
A kind of detection method of polymer polyatomic alcohol granularity, step is following:
(1) select 150 purpose stainless steel filtering nets, its size is length * wide * height: 5cm * 5cm * 2cm; Take by weighing 100 gram polymer polyatomic alcohol samples, be divided into two parts (being accurate to 0.1mg).
(2) measure the 100ml isopropanol solvent; A copy of it polymer polyatomic alcohol sample is diluted with isopropanol solvent; The sample good dilution filters with stainless steel filtering net, removes the good sample of dilution to topple over mode under field conditions (factors), makes liquid and passes through less than the particle of certain order number.
(3) dry together the particle that leaches with filter screen, placed 70 ℃～100 ℃ vacuum drying chambers dry 10 minutes.After being cooled to room temperature to sample and filter screen, take by weighing the content that calculates sample granularity.
Computing formula:
In the formula:
The granularity of X----sample, % (massfraction);
W
0The quality of----dry back solids and filter screen, g;
W
1The quality of-----sample, g;
W
2The quality of-----filter screen, g.
(4) according to step (2) and step (3) another part polymer polyatomic alcohol sample is detected equally.
(5) numerical value of twice mensuration is averaged, twice mensuration result's relative error is answered≤10PPm.
Embodiment 2:
Beyond distinguishing down, other are with embodiment 1.
(1) takes by weighing 60 gram polymer polyatomic alcohol samples, be divided into two parts (being accurate to 0.1mg).
(2) measure the 150ml alcohol solvent.
(3) the vacuum drying chamber temperature is 70～90 ℃, 5 minutes drying times.
Embodiment 3:
Beyond distinguishing down, other are with embodiment 1.
(1) takes by weighing 80 gram polymer polyatomic alcohol samples, be divided into two parts (being accurate to 0.1mg).
(2) measure the 200ml acetone solvent.
(3) the vacuum drying chamber temperature is 80～100 ℃, 15 minutes drying times.
Embodiment 4:
Beyond distinguishing down, other are with embodiment 1.
(1) takes by weighing 200 gram polymer polyatomic alcohol samples, be divided into two parts (being accurate to 0.1mg).
(2) measure the 300ml methanol solvate.
(3) the vacuum drying chamber temperature is 70～120 ℃, 20 minutes drying times.
This detection method is that polymer polyatomic alcohol provides favourable data, instructs the technological parameter prescription, makes the contradiction between polymer polyatomic alcohol product different quality index obtain optimum balance, so that the main functionality of outstanding polymer polyatomic alcohol product.Make the polymer polyatomic alcohol that makes possess stability, the finely divided advantage of low viscosity simultaneously; An important use of this polymer polyatomic alcohol is applicable to soft moulding and piece material and semi-hard polyurethane foam plastic; They can improve hardness and load-bearing capacity is improved, and this material also produces favorable influence to other performances of polyfoam such as beam drilling performance and anti-shrinkability.Obtained better technical effect.This method is other mensuration on year-on-year basis, and the method is stable, and more reliable, the result is more accurate.
Claims (10)
1. the detection method of a polymer polyatomic alcohol granularity; It is characterized in that; Processing step is: take by weighing said polymer polyatomic alcohol sample, with passing through strainer filtering behind the solvent dilution, place vacuum drying chamber to carry out drying together with filter screen the particle that leaches; Weigh after after drying finishes the particle that leaches and filter screen being cooled to room temperature, calculate the granularity of sample.
2. according to the detection method of the said polymer polyatomic alcohol granularity of claim 1, it is characterized in that said filter screen is selected the stainless steel material filter screen for use, its order number is 150 orders.
3. according to the detection method of the said polymer polyatomic alcohol granularity of claim 1, it is characterized in that said solvent is selected a kind of in isopropyl alcohol, ethanol, acetone or the methyl alcohol for use.
4. according to the detection method of the said polymer polyatomic alcohol granularity of claim 1, it is characterized in that the addition of said solvent is 100～300ml.
5. according to the detection method of the said polymer polyatomic alcohol granularity of claim 1, it is characterized in that the amount of taking by weighing of said polymer polyatomic alcohol sample is 1～100g.
6. according to the detection method of the said polymer polyatomic alcohol granularity of claim 5, it is characterized in that the amount of taking by weighing of said polymer polyatomic alcohol reagent is 30～50g.
7. according to the detection method of the said polymer polyatomic alcohol granularity of claim 1, it is characterized in that said drying box temperature is controlled at 70～120 ℃.
8. the detection method of said according to Claim 8 polymer polyatomic alcohol granularity is characterized in that, institute's drying box temperature is controlled at 70～90 ℃.
9. according to the detection method of the said polymer polyatomic alcohol granularity of claim 1, it is characterized in that be 5～30 minutes said drying time.
10. according to the detection method of the said polymer polyatomic alcohol granularity of claim 10, it is characterized in that be 5～10 minutes said drying time.
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| CN 201110243818 CN102323194B (en) | 2011-08-24 | 2011-08-24 | Detection method for particle size of polymer polyol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196802A (en) * | 2013-03-27 | 2013-07-10 | 中国矿业大学(北京) | Method for measuring and calculating radius-thickness ratio of laminated material for packing |
| CN112763383A (en) * | 2019-11-04 | 2021-05-07 | 乐凯华光印刷科技有限公司 | Method for measuring particle size and distribution of thermoplastic nano-micro particles by using photon-correlated nano-particle size analyzer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3813947A (en) * | 1972-01-11 | 1974-06-04 | Chamber Of Mines Services Ltd | Wet sieving |
| JPS5965240A (en) * | 1982-10-06 | 1984-04-13 | Mitsubishi Heavy Ind Ltd | Particle size measuring method |
| CN101949806A (en) * | 2010-09-21 | 2011-01-19 | 山东蓝星东大化工有限责任公司 | Novel detection method of solid content of polymer polyol |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3813947A (en) * | 1972-01-11 | 1974-06-04 | Chamber Of Mines Services Ltd | Wet sieving |
| JPS5965240A (en) * | 1982-10-06 | 1984-04-13 | Mitsubishi Heavy Ind Ltd | Particle size measuring method |
| CN101949806A (en) * | 2010-09-21 | 2011-01-19 | 山东蓝星东大化工有限责任公司 | Novel detection method of solid content of polymer polyol |
Non-Patent Citations (1)
| Title |
|---|
| 张玉春、度修孝、赵英华: "《中华人民共和国国家标准》", 1 October 1992 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196802A (en) * | 2013-03-27 | 2013-07-10 | 中国矿业大学(北京) | Method for measuring and calculating radius-thickness ratio of laminated material for packing |
| CN103196802B (en) * | 2013-03-27 | 2015-08-26 | 中国矿业大学(北京) | A kind of measuring method of filler sheet layer material radius-thickness ratio |
| CN112763383A (en) * | 2019-11-04 | 2021-05-07 | 乐凯华光印刷科技有限公司 | Method for measuring particle size and distribution of thermoplastic nano-micro particles by using photon-correlated nano-particle size analyzer |
| CN112763383B (en) * | 2019-11-04 | 2024-04-26 | 乐凯华光印刷科技有限公司 | Method for measuring particle size and distribution of thermoplastic nano-micron particles by using photon correlation nano-particle sizer |
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