CN111323334A - Method for testing foaming rate of solvent-free non-aqueous reaction type double-component foam polyurethane - Google Patents
Method for testing foaming rate of solvent-free non-aqueous reaction type double-component foam polyurethane Download PDFInfo
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- 238000005187 foaming Methods 0.000 title claims abstract description 86
- 238000012360 testing method Methods 0.000 title claims abstract description 46
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 33
- 239000004814 polyurethane Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000006757 chemical reactions by type Methods 0.000 title claims abstract description 15
- 239000006260 foam Substances 0.000 title claims description 25
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000007790 solid phase Substances 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000005357 flat glass Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000012935 Averaging Methods 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 3
- 239000011268 mixed slurry Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 230000000007 visual effect Effects 0.000 claims description 2
- 238000005070 sampling Methods 0.000 abstract description 7
- 230000007847 structural defect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 23
- 239000000463 material Substances 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000010998 test method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000007547 defect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000030944 contact inhibition Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/36—Analysing materials by measuring the density or specific gravity, e.g. determining quantity of moisture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/02—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by measuring weight of a known volume
- G01N9/04—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity by measuring weight of a known volume of fluids
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- Polyurethanes Or Polyureas (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention discloses a method for testing the foaming rate of solvent-free non-aqueous reaction type double-component foaming body polyurethane, which comprises the following steps: 1) preparing a foaming body; 2) preparing a standard sample; 3) measuring the mass, volume, solid phase density and average solid phase density of each standard sample; 4) calculating the foaming rate S, namely calculating the porosity of each standard sample, and processing all porosity data to obtain the average porosity; then calculating the ideal foaming total volume V3(ii) a Finally, according to the mixing volume V of the A, B components and the ideal foaming total volume V3And calculating to obtain the foaming rate. The method calculates the integral due volume of the foaming body according to the porosity of the part of the sample, solves the problem of low representativeness of the integral structure of the sample due to small sampling amount and structural defects, and has the advantages of simple and convenient operation and high accuracy.
Description
Technical Field
The invention relates to detection of physical properties of a polyurethane grouting material, in particular to a method for testing the foaming rate of a solvent-free non-aqueous reaction type double-component foam polyurethane.
Background
In recent years, polyurethane foam materials are often used in the field of underground engineering due to excellent water shutoff emergency performance, and the foaming rate is one of the main physical parameters of the materials, so that the foaming rate test is an essential link in scientific research and engineering application.
At present, the conventional method for testing the foaming rate of the polyurethane grouting material is divided into a method for testing the water-soluble (WPU) foaming rate and a method for testing the oil-soluble (OPU) foaming rate according to the type of the polyurethane material, and no matter what type of polyurethane, the foaming is generated after two components A, B are mixed, and the test process is as follows: weighing a certain amount of polyurethane in a 500mL (WPU) or 1000mL (OPU) container for foaming reaction, and calculating the whole foaming rate of the polyurethane by a water pouring mode after the foaming reaction is finished. As for the type of polyurethane material, the solvent-free non-aqueous reaction type two-component foaming polyurethane does not belong to the range of the two materials, the foaming reaction and the gel reaction of the reaction system have high speed, the heat release amount is large, the expansion stress in the reaction process is large, if the method is used for testing, the inhibition effect of a container on the volume increase of the container in the reaction process is more obvious compared with the other two materials, and the volume of a formed sample after foaming is smaller than the actual volume, so that the foaming rate is smaller.
In terms of sampling amount, the water-soluble polyurethane is 50g, the oil-soluble polyurethane is 25g, the size and the density distribution of pores of a sample obtained after reaction in a container are different, and the sample mainly comes from a plurality of factors such as side contact inhibition, reaction characteristics, interface effect and the like.
In order to make the foaming ratio test more scientific and objective, the sample preparation method and the foaming ratio test method need to be considered. Firstly, the solvent-free non-aqueous reaction type two-component polyurethane material has extremely high reaction rate, large reaction heat, fast strength rise (cooling is strength), and short forming time, so in the aspect of sample preparation, the structural uniformity and practical representativeness of a prepared sample need to be considered, and a common polyurethane sampling preparation method is not suitable for the reaction system, so that a mold and a test container need to be optimized in the aspect of sample preparation, and the prepared sample can reach an ideal foaming state as far as possible.
Secondly, the foaming rate is calculated by the traditional mode of using the sample in the water filling container as a whole, and because the precision of the container is tested and the interface influence is difficult to eliminate (for the test object, because the heat release is large, the speed is fast, the bottom contact surface cavity is large and the bottom structure is extremely uneven because the heat is not released in time), the obtained foaming rate is often not accurate enough and the accuracy is low.
In summary, the designed foaming ratio test method is required to have the following characteristics: 1) the general structural form of the sample is ensured to be consistent with the practical application of the material in the aspect of sampling and sample preparation, and the sample has practical representativeness; 2) the test method and the judgment standard are more fit with the actual physical properties of the solvent-free non-aqueous reaction type double-component foaming body polyurethane; 3) the test has strong operability and high accuracy.
Therefore, a foaming rate test method which is simple and convenient to operate and high in accuracy needs to be developed for the solvent-free non-aqueous reaction type two-component foaming polyurethane.
Disclosure of Invention
The invention aims to solve the defects of the background technology and provide a foaming rate test method which is developed aiming at the solvent-free non-aqueous reaction type two-component foaming polyurethane and has simple and convenient operation and high accuracy.
The technical scheme of the invention is as follows: a method for testing the foaming rate of solvent-free non-aqueous reaction type double-component foaming polyurethane is characterized by comprising the following steps:
1) preparation of the foam
Respectively weighing A, B components according to the proportion requirement, calculating the mixing volume V according to the mixing mass M of A, B components, rapidly stirring and uniformly mixing, pouring the mixed slurry onto plane glass to foam freely to form a foam body, and measuring the total mass M of the foam body1;
2) Preparation of Standard samples
Cutting the foaming body into 4 blocks from the center according to a cross, vertically cutting the same square section at the visually-observable uniformly-foaming position of each block to obtain 4 initial samples, cutting off the visually-observable non-uniformly-foaming positions at the top and the bottom of each initial sample to obtain 4 standard samples, and respectively marking as a standard sample A1、A2、A3、A4;
3) Measuring standard sample
Weighing standard sample A1、A2、A3、A4Mass m of1、m2、m3、m4And then measuring the volume V of each standard sample by using a wax sealing method1、V2、V3、V4Cutting off the contact part between the standard sample and wax, grinding the rest part into powder, and measuring by pycnometer method to obtain solid density rho1、ρ2、ρ3、ρ4And taking the average value to obtain the average solid phase density rho;
4) calculating the foaming ratio S
a. Firstly, according to the formula (1), calculating to obtain various standard samples AiPorosity n ofiAll porosities n are addediData ofThe treatment results in an average porosity n,
wherein, ViStandard sample AiVolume of (d), miStandard sample AiMass of (p;)iStandard sample AiI ═ 1, 2, 3, or 4;
b. then calculating according to the formula (2) to obtain the ideal foaming total volume V3,
Wherein M is1-total foam mass, ρ -average solid phase density, n-average porosity;
c. and finally, calculating according to the formula (3) to obtain the foaming ratio S:
wherein, V-mixing volume, V3-ideal total foamed volume.
Preferably, the mixing volume V in step 1) is the total mass M and the mixing density ρ0Calculated to obtain the mixing density rho0The volume of the A, B components is calculated by dividing the sum of the masses of the A, B components with the same proportion by the volume of the A, B components mixed and poured into a measuring cylinder quickly before the test.
Preferably, the mixing mass M of the A, B components in the step 1) is 80-100 g, and the stirring time is 15 s. The stirring time is set to be 15s, and the stirring time is obtained by comprehensively considering the reaction rate of the slurry reaction system and the uniformity of materials after reaction.
Preferably, the surface of the plate glass in the step 1) is clean and flat, the plate glass is placed stably without inclination, and drying treatment is carried out before the test.
Preferably, when the temperature of the foam to be foamed in the step 2) is cooled to 30-40 ℃, the foam is cut into 4 pieces from the center in a cross manner. The cutting and cooling temperature of the sample is set to be 30-40 ℃, so that the structure of the sample is prevented from being damaged (such as cracks and deformation) due to high-temperature cutting, and the phenomena of inconvenience in cutting or cutting loss due to high hardness of the material caused by low temperature are avoided.
Preferably, the vertical cuts in step 2) are made with square sections of 40mm by 40mm at the visual evenness of the individual pieces. The height h of the obtained standard sample is not less than 5 pore diameters.
Preferably, after the contact part of the surface of each standard sample and the wax is cut off in the step 3), the rest part is put into a planetary ball mill for crushing, the rotating speed of the planetary ball mill is set to be 300-400 r/min, and the ball milling medium is zirconia beads.
Preferably, in step 4), all porosities n are introducediThe method for obtaining the average porosity n by data processing comprises the following steps:
calculating each porosity niAnd all porosities niDeviation of the average value, the porosity is judged to be effective when the absolute value of the deviation is less than 10% of the average value of all porosities; when the porosity n is 4iAveraging all available porosities when at least 3 of them are available to obtain an average porosity n. If only two or one is effective, the test is repeated until 4 porosities n are obtainediAt least 3 of which are effective.
The invention sets the testing environment temperature (23 +/-2) DEG C, the relative humidity is less than 50 percent, the reaction is anhydrous reaction, and the influence of water on the reaction system is avoided as much as possible.
The invention has the beneficial effects that:
the invention designs a special foaming rate testing method aiming at the characteristics of high reaction rate, high reaction heat and excellent strength and rigidity after forming of a solvent-free non-aqueous reaction type double-component foaming body polyurethane material, optimizes a sampling mode, designs a more accurate testing mode, and reasonably establishes a judgment standard of the foaming rate testing method.
Secondly, the plane sample preparation method in the step 1) solves the defect that the side wall causes volume increase limitation in a conventional foaming rate test, and simultaneously, the heat at the bottom of the sample is released more quickly due to the disappearance of side resistance and the increase of the cross section of the sample, so that the bottom defect caused by heat accumulation is reduced, and the uniformity of the whole structure of the sample is enhanced; in the step 2), the sample is selectively cut, so that the influence of uneven size distribution of air holes at the bottom and other edges on the experiment is eliminated, and the structural representativeness of the sample is further enhanced;
comparing the mode of calculating the foaming rate by testing the porosity of the material in the step 4) with the traditional method of calculating the foaming rate by water filling, the method has two advantages: 1. the porosity test of the sample is from the angle of the internal structure of the sample, a structure is selected to represent a main structure of the sample in actual large-dose use, the measured porosity is high in representativeness, the porosity of the sample is used for calculating the due volume of the sample in the structure, the problem that the representativeness of the whole structure of the sample is not high due to small sampling amount and structural defects is solved, and therefore the accuracy of calculating the foaming rate by using the porosity is high; 2. in terms of the test process, the selected instrument and the gauge have higher accuracy, and the obtained result has higher accuracy.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Examples
The invention provides a method for testing the foaming rate of solvent-free non-aqueous reaction type double-component foaming body polyurethane, which comprises the following steps:
1) preparation of the foam
A, B components, 40.8g of A component, 39.2g of B component, 80g of mixed mass M and mixed density rho are weighed according to the proportioning requirement0=1.120g/mL(ρ0Dividing the mass sum of A, B components with the same proportion by the volume obtained by mixing the A, B components and quickly pouring the A, B components into a measuring cylinder before testing), calculating to obtain a mixed volume V which is 71.43mL, pouring A, B components into a mixing beaker simultaneously, quickly mixing and stirring for 15s, pouring the mixed slurry onto flat glass for free foaming, wherein the pouring speed is not too high, ensuring that the slurry starts to react within 6s after pouring is finished, foaming is finished to form a foaming body, the size of the flat glass is 50cm to 50cm, the surface is clean and flat, the flat glass is placed stably without inclination, drying before testing, and measuring the total mass M of the foaming body1=73.80g;
2) Preparation of Standard samples
Cutting the foaming body into 4 blocks from the center according to a cross shape when the temperature of the foaming body is cooled to be between 30 and 40 ℃, vertically cutting the visually-measured uniformly-foamed part of each block at a square section of 40 mm-40 mm to obtain 4 initial samples, cutting off the visually-measured non-uniformly-foamed part at the top and the bottom of each initial sample to obtain a standard sample (the height h of the standard sample is not less than 5 pore diameters), and marking the standard sample as a standard sample A1、A2、A3、A4;
3) Measuring standard sample
Weighing standard sample A1、A2、A3、A4Mass m of1、m2、m3、m4And then measuring the volume V of each standard sample by using a wax sealing method1、V2、V3、V4The standard sample A1、A2、A3、A4After the surface is wiped dry, the part contacting with the wax is cut off, the rest part is put into a planetary ball mill for crushing, the rotating speed of the planetary ball mill is set to be 300-400 r/min, the time is 1h, the ball milling medium is zirconia beads, and the obtained powder is measured by a pycnometer method to obtain the solid phase density rho1、ρ2、ρ3、ρ4All solid phase densities ρ1、ρ2、ρ3、ρ4Taking the average value to obtain the average solid phase density rho, wherein the obtained data are shown in the following table 1;
4) calculating the foaming ratio S
a. Firstly, according to the formula (1), calculating to obtain various standard samples A1、A2、A3、A4Porosity n of1、 n2、n3、n4All porosities n are added1、n2、n3、n4And (3) processing the data to obtain the average porosity n, wherein when the data are processed: calculating each porosity n1、n2、n3、n4And (n)1+n2+n3+n4) A deviation of/4 in absolute value of the deviation less than (n)1+n2+n3+n4) 10% of/4 judged the porosity as valid;when the porosity n is 41、n2、n3、n4Averaging all available porosities when at least 3 of them are available to obtain an average porosity n. If only two or one are effective, the trial is repeated until at least 3 of the 4 porosities are effective. All porosities are judged to be effective in this example, so the average porosity n is n1、n2、n3、n4Average value of, obtained n1、n2、n3、n4And n data as shown in table 1,
wherein n isiStandard sample AiPorosity of, ViStandard sample AiVolume of (d), miStandard sample AiMass of (p;)iStandard sample AiI ═ 1, 2, 3, or 4;
b. then calculating according to the formula (2) to obtain the ideal foaming total volume V3,
Wherein M is1=73.80g、ρ=1.164g/cm3、n=87.7%,
Thereby V3=515.46cm3;
c. And finally, calculating according to the formula (3) to obtain the foaming ratio S:
wherein, V is 71.43mL and V3=515.46cm3And thus S-622%.
Table 1 standard sample data table
Comparative example 1
According to the content of the foaming rate test method of the conventional water-soluble (WPU) polyurethane grouting material, the foaming rate test (the water adding link before the reaction is removed) is carried out on the same test material in the embodiment, A, B slurry with the total mass of 50g is weighed and placed in 500mL for test, the initial volume of the obtained material is 44.64mL, the irrigation volume is 254.48mL, and the foaming rate is 450% by calculation.
Comparative example 2
The foaming rate test (except for the water addition step before the reaction) was carried out on the same test materials in the examples according to the content of the foaming rate test method of the conventional oil soluble (OPU) polyurethane grouting material, wherein A, B slurry with a total mass of 25g was weighed and placed in 1000mL for testing, and the foaming rate was 570% by calculation with an initial volume of 22.32mL and a water injection volume of 850.46 mL.
TABLE 2 foaming ratio comparison data sheet
The invention | Comparative example 1 | Comparative example 2 | |
Foaming ratio (%) | 622 | 450 | 570 |
As can be seen from Table 1, Standard A1、A2、A3、A4The measured solid density and porosity data have small difference, which shows that the sample prepared by the designed sampling method has good structural homogeneity and is suitable for the polymerization of the reaction systemThe preparation method of the polyurethane material sample simultaneously utilizes the porosity of the representative structure to calculate the overall porosity, and the result obtained by calculating the overall porosity has high accuracy; as can be seen from Table 2, the foaming ratios of comparative examples 1 and 2 are smaller than those of the examples of the invention, which shows that the inhibition effect of the contact surface has great influence on the volume increase of the tested object, particularly, the comparative example 1 has smaller container volume and stronger inhibition effect performance, and the invention directly avoids the defect, and utilizes the representative structure to directly test the physical properties of the material so as to locally calculate the whole body, thereby having high feasibility.
Claims (8)
1. A method for testing the foaming rate of solvent-free non-aqueous reaction type double-component foaming polyurethane is characterized by comprising the following steps:
1) preparation of the foam
Respectively weighing A, B components according to the proportion requirement, calculating the mixing volume V according to the mixing mass M of A, B components, rapidly stirring and uniformly mixing, pouring the mixed slurry onto plane glass to foam freely to form a foam body, and measuring the total mass M of the foam body1;
2) Preparation of Standard samples
Cutting the foaming body into 4 blocks from the center according to a cross, vertically cutting the same square section at the visually-observable uniformly-foaming position of each block to obtain 4 initial samples, cutting off the visually-observable non-uniformly-foaming positions at the top and the bottom of each initial sample to obtain 4 standard samples, and respectively marking as a standard sample A1、A2、A3、A4;
3) Measuring standard sample
Weighing standard sample A1、A2、A3、A4Mass m of1、m2、m3、m4And then measuring the volume V of each standard sample by using a wax sealing method1、V2、V3、V4Removing the contact part between the standard sample and the wax, grinding the rest part into powder, and measuring by a pycnometer method to obtain the solid density rho of each standard sample1、ρ2、ρ3、ρ4And taking the average value to obtain the average solid phase density rho;
4) calculating the foaming ratio S
a. Firstly, according to the formula (1), calculating to obtain various standard samples AiPorosity n ofiAll porosities n are addediThe data is processed to obtain the average porosity n,
wherein, ViStandard sample AiVolume of (d), miStandard sample AiMass of (p;)iStandard sample AiI ═ 1, 2, 3, or 4;
b. then calculating according to the formula (2) to obtain the ideal foaming total volume V3,
Wherein M is1-total foam mass, ρ -average solid phase density, n-average porosity;
c. and finally, calculating according to the formula (3) to obtain the foaming ratio S:
wherein, V-mixing volume, V3-ideal total foamed volume.
2. The method for testing the foaming ratio of the solventless, nonaqueous reactive two-component foam polyurethane according to claim 1, wherein the mixing volume V in the step 1) is the mixing mass M and the mixing density ρ0Calculated to obtain the mixing density rho0The volume of the A, B components is calculated by dividing the sum of the masses of the A, B components with the same proportion by the volume of the A, B components mixed and poured into a measuring cylinder quickly before the test.
3. The method for testing foaming rate of solventless nonaqueous reaction type two-component foam polyurethane as claimed in claim 1, wherein the mixing mass M of the A, B component in the step 1) is 80-100 g, and the stirring time is 15 s.
4. The method for testing the foaming ratio of the solvent-free non-aqueous reactive two-component foam polyurethane as claimed in claim 1, wherein the surface of the plate glass in the step 1) is clean and flat, the plate glass is placed stably without inclination, and the plate glass is dried before the test.
5. The method for testing the foaming ratio of the solventless, nonaqueous reactive two-component foam polyurethane as claimed in claim 1, wherein the foam is cut into 4 pieces from the center in a cross shape when the temperature of the foam to be foamed in step 2) is cooled to 30 to 40 ℃.
6. The method for testing the foaming ratio of the solvent-free non-aqueous reactive two-component foam polyurethane according to claim 1, wherein the vertical cutting is performed at a square section of 40mm x 40mm at the visual uniform foaming of each block in the step 2).
7. The method for testing the foaming ratio of the solventless nonaqueous reaction type two-component foam polyurethane according to claim 1, wherein the surface of each standard sample in step 3) is partially cut off after contacting with the wax, the remaining part is crushed in a planetary ball mill, the planetary ball mill is set to rotate at a speed of 300 to 400r/min, and the ball milling medium is zirconia beads.
8. The method for testing the foaming ratio of the solventless, nonaqueous reactive two-component foam polyurethane according to claim 1, wherein in the step 4), all the porosities n are measurediThe method for obtaining the average porosity n by data processing comprises the following steps: calculating each porosity niAnd all porosities niDeviation of the average value, the porosity is judged to be effective when the absolute value of the deviation is less than 10% of the average value of all porosities; when the porosity n is 4iAveraging all available porosities when at least 3 of them are available to obtain an average porosity n.
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CN112924336A (en) * | 2021-02-01 | 2021-06-08 | 郑州大学 | Method for testing and verifying dissolution curve of double-component high polymer physical foaming agent |
CN115071036A (en) * | 2022-07-19 | 2022-09-20 | 中国汽车技术研究中心有限公司 | Method, equipment and storage medium for preprocessing raw materials of skin and muscle layers of collision dummy |
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