CN112924335B - Method for testing dissolution curve of physical foaming agent in single-component high polymer - Google Patents

Method for testing dissolution curve of physical foaming agent in single-component high polymer Download PDF

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CN112924335B
CN112924335B CN202110135832.4A CN202110135832A CN112924335B CN 112924335 B CN112924335 B CN 112924335B CN 202110135832 A CN202110135832 A CN 202110135832A CN 112924335 B CN112924335 B CN 112924335B
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foaming agent
slurry
physical foaming
time
calculating
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CN112924335A (en
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李晓龙
贾赫扬
钟燕辉
张蓓
李阳
潘艳辉
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Henan Research Institute Of Sun Yat Sen University
Zhengzhou University
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Henan Research Institute Of Sun Yat Sen University
Zhengzhou University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N2013/006Dissolution of tablets or the like

Abstract

The invention provides a method for testing the dissolution curve of a physical foaming agent in a single-component polymer, which comprises the steps of heating polymer slurry in which the physical foaming agent is dissolved, recording temperature values and liquid level height values of the polymer slurry at different moments, calculating the volume value of the slurry at the corresponding moment according to the liquid level height value, calculating the solubility of the physical foaming agent at different temperatures according to the temperature and the volume of the polymer slurry to obtain a curve of the solubility of the physical foaming agent along with the temperature change, and finally verifying the applicability of the measured solubility curve of the physical foaming agent through the comparison of a foaming test of the polymer slurry and a numerical simulation result. The invention compares the analog value with the test value by using temperature and density, and then is more consistent, thereby proving the accuracy and the rationality of the solubility curve.

Description

Method for testing dissolution curve of physical foaming agent in single-component high polymer
Technical Field
The invention belongs to the field of chemical grouting, and particularly relates to a method for testing a dissolution curve of a physical foaming agent in a single-component high polymer.
Background
The single-component high polymer grouting material has the characteristics of reaction in water, quick expansion, early strength, water resistance and the like, and is widely applied to seepage-proofing reinforcement engineering in the fields of water conservancy, traffic, mining and the like.
The research on the diffusion mechanism of the single-component high polymer slurry has important guiding significance for grouting design and construction. Simulating the expansion diffusion process of the high polymer by means of simulation is an important way for researching the diffusion mechanism of the high polymer slurry. After the high polymer is injected, the high polymer quickly undergoes chemical reaction when meeting field water, a large amount of heat energy is released, the temperature of the slurry is continuously increased, and the physical foaming agent is gradually gasified to form a large amount of micro closed-cell bubbles which are suspended in the slurry, so that the volume of the slurry is continuously expanded, and the slurry is driven to flow. Therefore, in order to research the diffusion mechanism of the high polymer, the expansion process of the high polymer slurry needs to be accurately solved, and the key point is to master a solubility model of the physical foaming agent in the high polymer slurry.
Different types of physical foaming agents have different solubility properties in different polymer slurries, so for any physical foaming agent, a pertinence test needs to be performed according to the type of the polymer slurry dissolved in the physical foaming agent to obtain a corresponding solubility curve, however, a quick and efficient calculation method for the solubility curve of the physical foaming agent in the polymer slurry is lacked at present.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a method for testing the dissolution curve of a physical foaming agent in a single-component high polymer, which comprises the steps of heating high polymer slurry in which the physical foaming agent is dissolved, recording temperature values and liquid level height values of the high polymer slurry at different moments, calculating the volume value of the slurry at the corresponding moment according to the liquid level height values, and then calculating the solubility of the physical foaming agent at different temperatures according to the temperature and the volume of the high polymer slurry to obtain the change curve of the solubility of the physical foaming agent along with the temperature.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for testing the dissolution curve of a physical foaming agent in a single-component high polymer comprises the following steps:
s1, heating and dissolving high polymer slurry containing a physical foaming agent, reading and recording temperature values and liquid level height values of the high polymer slurry at different moments, and calculating the volume V (t) of the slurry at the moment t according to the liquid level height values;
s2, according to the volume V of the slurry at the initial moment 0 And the volume V (t) of the slurry obtained in the step S1, and calculating gas at the t moment by using an ideal gas equationThe mole number n of the chemical part of the physical foaming agent;
s3, calculating the mass m of the gasified partial physical foaming agent at the time t by using a molar mass formula according to the molar number n obtained in the step S2 BG
S4, utilizing the mass m of the partial physical foaming agent gasified at the time t obtained in the step S3 BG Calculating the solubility r of the physical foaming agent in the component B slurry at the time t according to a solubility formula BL
And S5, repeating the steps S1 to S4, calculating the solubility of the physical foaming agent at the corresponding temperature at different moments, and performing data fitting in an exponential function mode to obtain a curve of the solubility of the physical foaming agent along with the change of the temperature.
In a preferred embodiment, the step S1 specifically includes:
s11: injecting high polymer slurry containing a physical foaming agent into a graduated measuring cylinder;
s12: placing the temperature sensor in a measuring cylinder, and immersing a probe of the temperature sensor in the slurry;
s13: placing the measuring cylinder in the step S12 on a heating device for heating;
s14: reading and recording temperature values T of the slurry at different moments in the heating process;
s15: reading the height value of the highest point of the slurry surface on the measuring cylinder and the corresponding height value of the regular liquid level according to
Figure BDA0002926914180000021
The volume V (t) of the slurry at time t is calculated,
in the above formula, R is the radius, h (t) is the height from the bottom to the highest point of the liquid level at the moment t, h 1 (t) is the height from the bottom to the lowest point of the liquid surface at time t.
In a preferred embodiment, the step S2 specifically includes:
s21, volume V (t) of the slurry according to time t and volume V of the slurry at initial time 0 Determining the volume Δ V, Δ V = V (t) -V of the physical blowing agent vaporized at time t 0
And S22, calculating the mole number n of the gasified physical foaming agent according to the delta V and an ideal gas equation p delta V = nRT, wherein p is the atmospheric pressure, R is a Prov gas constant and is 8.31J/(mol · k), and T is the slurry temperature at the time T.
In a preferred embodiment, the step S3 is specifically:
according to the molar number n and the molar mass formula m BG =n×M B Calculating to obtain the mass m of the physical foaming agent of the gasified part at the time t BG Wherein M is B Is the physical blowing agent molar mass.
In a preferred embodiment, the step S4 is specifically:
according to m BG And solubility formula
Figure BDA0002926914180000031
Calculating to obtain the solubility r of the physical foaming agent in the slurry BL Wherein m is the total mass of the polymer slurry, m B Is the total mass of the physical blowing agent.
In a preferred embodiment, the polymer slurry comprises a polyol, a chemical blowing agent, a physical blowing agent, a catalyst.
In a preferred embodiment, the physical blowing agent comprises one of monofluorotrichloromethane, monofluorotrichloroethane, trifluoromonochloromethane, monofluorodichloroethane, cyclopentane.
The invention has the following beneficial effects:
the invention provides a method for testing a dissolution curve of a two-component high polymer physical foaming agent, which comprises the steps of heating high polymer slurry dissolved with the physical foaming agent, recording temperature values and liquid level height values of the high polymer slurry at different moments, calculating volume values of the slurry at corresponding moments according to the liquid level height values, calculating the solubility of the physical foaming agent at different temperatures according to the temperature and the volume of the high polymer slurry, and performing data fitting in an exponential function mode to obtain a curve of the solubility of the physical foaming agent along with the change of the temperature, thereby providing an important way for researching the diffusion mechanism of the high polymer.
Drawings
FIG. 1 is a plot of the temperature of a polymer slurry over time in example 1 of the present invention;
FIG. 2 is a plot of polymer slurry volume as a function of time for example 1 in accordance with the present invention;
FIG. 3 is a plot of the solubility of the polymer slurry in example 1 of the present invention as a function of temperature.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the description herein, reference to the description of the terms "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The polyol and catalyst in the polymer slurry in this embodiment are not limited, and may be any polyol and catalyst that can be used in the existing polymer mixture, the chemical blowing agent is water, and the physical blowing agent is cyclopentane. Physical property in high polymer slurry at initial timeMass m of blowing agent B 7.20g, the initial polymer slurry mass m was 372g, the initial temperature was 26.5 ℃ and the initial polymer slurry volume was 150cm 3 The standard atmospheric pressure p is 1.01325X 10 5 Pa。
A method for calculating the dissolution curve of a physical foaming agent in a single-component high polymer comprises the following steps:
s1, heating and dissolving high polymer slurry containing a physical foaming agent, reading and recording temperature values and liquid level height values of the high polymer slurry at different moments, and calculating the volume V (t) of the slurry at the moment t according to the liquid level height values.
The specific method comprises the following steps:
s11: injecting high polymer slurry containing a physical foaming agent into a graduated measuring cylinder;
s12: placing the temperature sensor in a measuring cylinder, and immersing a probe of the temperature sensor in the slurry;
s13: placing the measuring cylinder in the step S12 on a heating device for heating;
s14: reading and recording temperature values T of the slurry at different moments in the heating process, wherein the result is shown as a curve of the temperature of the high polymer slurry changing along with time in figure 1, and the temperature of the high polymer slurry also gradually increases along with the increase of the time;
s15: reading the height value of the highest point of the slurry surface on the measuring cylinder and the height value corresponding to the regular liquid surface according to
Figure BDA0002926914180000041
The volume V (t) of the slurry at time t is calculated,
in the above formula, R is the radius, h (t) is the height from the bottom to the highest point of the liquid level at the moment t, h 1 (t) is the height from the bottom to the lowest point of the liquid surface at time t, and as shown in FIG. 2, it can be seen from FIG. 2 that the volume does not change significantly at the initial stage of the reaction and then rises sharply.
S2, according to the volume V of the slurry at the initial moment 0 And the volume V (t) of the slurry obtained in step S1, and calculating the mole number n of the gasified partial physical foaming agent at the time t by using an ideal gas equation.
The specific method comprises the following steps:
s21, volume V (t) of the slurry according to time t and volume V of the slurry at initial time 0 Determining the volume Δ V, Δ V = V (t) -V of the physical blowing agent vaporized at time t 0
And S22, calculating the mole number n of the gasified physical foaming agent according to the delta V and an ideal gas equation p delta V = nRT, wherein p is the atmospheric pressure, R is a Poisson' S gas constant and is 8.31J/(mol · k), and T is the slurry temperature at the time T.
S3, calculating the mass m of the gasified partial physical foaming agent at the time t by using a molar mass formula according to the molar number n obtained in the step S2 BG
Concretely, the method is based on a molar number n and a molar mass formula m BG =n×M B Calculating to obtain the mass m of the physical foaming agent of the gasified part at the time t BG Wherein M is B Is the physical blowing agent molar mass.
S4, utilizing the mass m of the partial gasified physical foaming agent at the time t obtained in the step S3 BG Calculating the solubility r of the physical foaming agent in the component B slurry at the t moment according to a solubility formula BL
According to m BG And solubility formula
Figure BDA0002926914180000051
Calculating to obtain the solubility r of the physical foaming agent in the slurry BL Wherein m is the total mass of the B component slurry, m B Is the total mass of the physical blowing agent.
And S5, repeating the steps S1-S4, recording the solubility of the physical foaming agent at the corresponding temperature at different moments, and performing data fitting in an exponential function mode to obtain a curve of the solubility of the physical foaming agent along with the change of the temperature.
The solubility model of the physical blowing agent in the self-expanding polymer slurry obtained according to this example is:
Figure BDA0002926914180000052
wherein, a = -2.67781 × 10 -5 ,b=0.02725,c=-7.26908×10 -6 D =0.00478, e =0.75947. As a result, as shown in FIG. 3, the solubility gradually decreased with time at the initial stage of the reaction, and the change was not significant, and then the solubility decreased sharply with the increase in temperature.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and is not intended to limit the practice of the invention to these embodiments. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (4)

1. A method for testing the dissolution curve of a physical foaming agent in a single-component high polymer is characterized by comprising the following steps:
s1, heating and dissolving high polymer slurry containing a physical foaming agent, reading and recording temperature values and liquid level height values of the high polymer slurry at different moments, and calculating the volume V (t) of the slurry at the moment t according to the liquid level height values;
s2, calculating the mole number n of the gasified partial physical foaming agent at the time t by using an ideal gas equation according to the volume V0 of the slurry at the initial time and the volume V (t) of the slurry obtained in the step S1, wherein the step S2 specifically comprises the following steps:
s21, obtaining the volume delta V of the physical foaming agent gasified at the time t according to the volume V (t) of the slurry at the time t and the volume V0 of the slurry at the initial time, wherein the delta V = V (t) -V0;
s22, calculating the mole number n of the gasified physical foaming agent according to the delta V and an ideal gas equation p delta V = nRT, wherein p is atmospheric pressure, R is a Poisson' S gas constant and is 8.31J/(mol · k), and T is the slurry temperature at the time T;
s3, calculating the mass mBG of the gasified partial physical foaming agent at the time t by using a molar mass formula according to the molar number n obtained in the step S2;
s4, calculating the solubility rBL of the physical foaming agent in the polymer slurry at the time t according to a solubility formula by using the mass mBG of the gasified part of the physical foaming agent at the time t obtained in the step S3, wherein the step S4 specifically comprises the following steps:
according to the mBG and solubility formula r BL =(m B -m BG )/(m-m B ) Calculating to obtain the solubility r of the physical foaming agent in the slurry BL Wherein m is the total mass of the polymer slurry, m B Is the total mass of physical blowing agent;
and S5, repeating the steps S1-S4, calculating the solubility of the physical foaming agent at the corresponding temperatures at different moments, and performing data fitting in an exponential function mode to obtain a curve of the solubility of the physical foaming agent along with the change of the temperature, wherein the physical foaming agent comprises one of fluorotrichloromethane, fluorotrichloroethane, trifluoromonochloromethane, fluorodichloroethane and cyclopentane.
2. The method for testing the dissolution curve of a physical blowing agent in a single-component polymer according to claim 1, wherein the step S1 specifically comprises:
s11: injecting high polymer slurry containing a physical foaming agent into a graduated measuring cylinder;
s12: placing the temperature sensor in a measuring cylinder, and immersing a probe of the temperature sensor in the slurry;
s13: placing the measuring cylinder in the step S12 on a heating device for heating;
s14: reading and recording temperature values T of the slurry at different moments in the heating process;
s15: reading the height value of the highest point of the liquid level of the slurry on the measuring cylinder and the corresponding height value of the regular liquid level according to
Figure FDA0004021483310000021
Calculating the volume V (t) of the slurry at the time t,
in the above formula, R is the radius, h (t) is the height from the bottom to the highest point of the liquid surface at the time t, and h1 (t) is the height from the bottom to the lowest point of the liquid surface at the time t.
3. The method for testing the dissolution curve of the physical foaming agent in the single-component polymer according to claim 1, wherein the step S3 is specifically:
and calculating the mass mBG of the gasified part of the physical foaming agent at the time t according to the molar number n and a molar mass formula mBG = n × MB, wherein MB is the molar mass of the physical foaming agent.
4. The method for testing the dissolution curve of a physical blowing agent in a single component polymer according to any one of claims 1 to 3, wherein the polymer slurry comprises a polyol, a chemical blowing agent, a physical blowing agent, and a catalyst.
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