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CN115246916B - Preparation method of high-flux homogeneous solid phase extraction disc - Google Patents

Preparation method of high-flux homogeneous solid phase extraction disc Download PDF

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CN115246916B
CN115246916B CN202211027641.7A CN202211027641A CN115246916B CN 115246916 B CN115246916 B CN 115246916B CN 202211027641 A CN202211027641 A CN 202211027641A CN 115246916 B CN115246916 B CN 115246916B
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polyol
phase extraction
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surfactant
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CN115246916A (en
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韩杰
邱维
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Xixian New Area Guyiheng Technology Co ltd
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Xixian New Area Guyiheng Technology Co ltd
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    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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Abstract

The invention discloses a preparation method of a high-flux homogeneous solid-phase extraction disc, which comprises the steps of preparing a polyol mixed solution by taking a polyol system, a foaming agent and a surfactant as raw materials, adding isocyanate, uniformly mixing, continuously stirring until the system reaches a milky state, pouring into a mould for solidification until the system is solidified completely, obtaining a polyurethane soft foam material, and dividing the polyurethane soft foam material according to the standard size and thickness of the solid-phase extraction disc, thus obtaining the high-flux homogeneous solid-phase extraction disc. The high-flux homogeneous solid phase extraction disk prepared by the preparation method has high flux and small solvent consumption, can be used for detecting samples with complex components, and has lower cost than the solid phase extraction disk in the prior art.

Description

Preparation method of high-flux homogeneous solid phase extraction disc
Technical Field
The invention belongs to the technical field of consumable materials of chemical analysis testing instruments, and relates to a preparation method of a high-flux homogeneous solid phase extraction disc.
Background
At present, the quantitative analysis of pollutants in environmental water body needs pretreatment of raw water samples, and the treatment methods mainly comprise liquid-liquid extraction (LLE), solid Phase Extraction (SPE), solid Phase Microextraction (SPME) and the like. Among them, solid Phase Extraction (SPE) is most widely used in practice. The technology is based on the distribution behavior of target analytes in liquid-solid phases, adopts solid adsorbent, solvent elution and other modes to selectively enrich, separate and purify the target analytes in the sample. Compared with the traditional liquid-liquid extraction (LLE), the solid phase extraction technology has the advantages of less solvent consumption, high enrichment factor, convenient operation and use and the like. As a convenient technology for separating and enriching target analytes in samples, the solid phase extraction technology is widely applied to detection of trace analytes in water, and becomes an important tool in the fields of environmental water sample analysis, food and beverage, pharmacy, quality control method detection and scientific research.
The common solid phase extraction consumable material comprises a solid phase extraction column and a solid phase extraction disc, and the solid phase extraction column is suitable for processing small-volume samples in a laboratory due to low sample flux and complex device, and is not suitable for field operation or large-volume sample processing (such as environmental water samples). The existing solid-phase extraction discs in the market solve the problems of low flow speed, ditch flow and easy blockage of the traditional extraction columns to a certain extent, but the products have complex manufacturing process and high cost, and the sample flux and the manufacturing process are limited by the complex structure of the fiber membrane matrix embedded adsorbent particles. Taking EMPORE series of solid phase extraction discs produced by the original 3M company as an example, the series of products are representative products of the solid phase extraction discs in the field of global solid phase extraction, and the application is the most widely. However, this series of products has the following problems in practical applications: (1) flux limitation: the solid phase extraction material encapsulated inside EMPORE membranes is porous adsorbent particles with a diameter of about 12 microns. This configuration determines that the effective pore size of the membrane for the sample to pass through is below a few microns to avoid loss of adsorbent particles with the sample during use of the product. This structure results in a EMPO RE membrane sample throughput that does not overcome the current bottleneck. (2) solvent consumption: the EMPORE series of solid phase extraction membranes are composed of polytetrafluoroethylene fiber membranes with high hydrophobicity and hydrophobic porous adsorbents (porous adsorbent particles such as C18/C8 bonded silica gel, SDB-XC/SDB-RPS adsorption resin and the like) encapsulated in the membranes. Before injection, the sample needs to be soaked with organic solvent repeatedly for a plurality of times (commonly called as activation). This processing step is critical to ensure recovery and reproducibility of the results of the target analyte in the sample and therefore requires strict performance in operation. However, this step requires about 100mL of high purity organic solvent (for example, a EMPORE solid phase extraction disk with a diameter of 47 mm) to generate unnecessary laboratory waste liquid and additional time for the laboratory operator. (3) complex component samples are difficult to process: EMPORE the solid phase extraction membrane adopts a porous adsorbent as its solid phase extraction medium. Taking the most commonly used C18, SDB-XC type solid phase extraction discs for organic pollutants as an example, the selectivity of the adsorbent for the components in the sample is limited only by the hydrophilicity and hydrophobicity of the compound itself. For samples with complex components, competitive adsorption between coexisting substances and analytes is easy to occur in the solid-phase extraction process, so that the extraction agent is saturated and penetrated prematurely, and the recovery rate and purity of target analytes in the samples are directly affected. In addition, because EMPO RE membranes have a small pore size, samples containing soluble polymers must be prefiltered before they can be loaded, otherwise the sample throughput during extraction can be too low or the membranes can be quickly plugged. (4) expensive materials: the single use of solid phase extraction consumables makes it a major cost item in this technology application. EMPORE has a selling price which is about 3-10 times that of the solid-state extraction column with the same purpose, and the high selling price greatly increases the consumable use cost of the solid-state extraction technology, so that the low-flux traditional solid-state extraction column can compete with the solid-state extraction column with the high-cost solid-state extraction column in the market for a long time. In addition to technical monopolization and lack of product competition, the high price of solid-phase extraction disk products is also determined by its own structure and complex manufacturing process. Solid phase extraction membrane products (including EMPORE series produced by original 3M company, american Agilent SPEC series, american Restek Resprep series, swedish Biotage Atlantic series and French AFFINISEP ATTRACTSPE series) in the market all adopt a two-phase composite structure of membrane internally packaged micron-sized adsorbent particles, and the product has a complex structure and high manufacturing and processing barriers.
Aiming at the problems, the invention provides a preparation method of a high-flux homogeneous solid phase extraction disc.
Disclosure of Invention
The invention aims to provide a preparation method of a high-flux homogeneous solid-phase extraction disc, which realizes high-flux and selective solid-phase extraction and solves the problems that the solid-phase extraction disc prepared by the preparation method in the prior art is limited in flux, high in solvent consumption, difficult to process samples with complex components, high in selling price and the like in practical application.
The technical scheme adopted by the invention is that the preparation method of the high-flux homogeneous solid phase extraction disc is implemented according to the following steps:
Step 1, weighing polyol, foaming agent, surfactant, catalyst and additive, wherein the addition amount of the foaming agent is 3-30% of the mass of the polyol, the addition amount of the surfactant is 2-3% of the mass of the polyol, the addition amount of the catalyst is 1-2% of the mass of the polyol, and the addition amount of the additive is 1-10% of the mass of the polyol;
Step 2, mixing the polyol, the foaming agent, the surfactant, the catalyst and the additive which are weighed in the step 1, and stirring for 5-25min at a rotating speed of 1500-2500 r/min to uniformly mix the components, so as to obtain a polyol mixed solution;
Step 3, adding isocyanate into the polyol mixed solution obtained in the step 2, and stirring at a rotating speed of 1000-6000 r/min for 10-60 s to uniformly mix the isocyanate and the polyol mixed solution to obtain a mixture A;
Step 4, continuously stirring the mixture A at a rotating speed of 1000-6000 r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
The present invention is also characterized in that,
The polyol in the step 1 adopts polyester, polyether or other alcohols with two or more hydroxyl groups, specifically any one of polypropylene glycol, trihydroxy polyether, polyoxypropylene glycol, polyester polyol, polycaprolactone polyol or polycarbonate diol.
The foaming agent in the step 1 adopts any one of dichloromethane, trifluoromethane, n-pentane or distilled water.
The surfactant in the step 1 adopts any one of organosilicon surfactant, polyether modified organosilicon surfactant, polysiloxane-polyoxyalkylene ether block copolymer or silicone oil.
The catalyst in the step 1 adopts any one of triethylenediamine, tin octoate or dibutyltin dilaurate.
The additive in the step 1 is any one of a pore opening agent, a foam stabilizer and a chain extender.
The isocyanate used in step 3 has two or more isocyanate functional groups, specifically any one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate or polymethylene diphenyl diisocyanate. The addition amount of the isocyanate is 100-300% of the mass of the polyol. The amount of isocyanate added is required to be in accordance with the isocyanate index R, i.e., the molar ratio of-NCO in the isocyanate to-OH in the polyol is from 0.8 to 1.2.
The beneficial effects of the invention are as follows:
the invention relates to a preparation method of a high-flux homogeneous solid-phase extraction disc, which adopts a polymer disc with molecular absorption capacity and an open pore self-supporting structure to realize high-flux and selective solid-phase extraction and solve a plurality of bottleneck problems of the solid-phase extraction disc in practical application:
(1) The invention abandons the complex two-phase structure of packaging micron-sized adsorbent particles in a fiber membrane commonly adopted by a solid-phase extraction membrane, utilizes the absorption effect of polyether polyurethane sponge on dissolved organic molecules in water and the intrinsic characteristics thereof and the apparent distribution behavior rule of compounds in two phases of sponge fibers and water, autonomously develops a polymer with selective molecular absorption capacity as a homogeneous phase extraction medium, has a self-supporting framework and no dead volume, and realizes the integration of the membrane extraction medium and a supporting material;
(2) The solid phase extraction disc provided by the invention is a homogeneous phase open pore material, and the material itself has an open pore structure with high porosity and adjustable size, and micron-sized adsorbent particles do not need to be packaged in the structure. The thickness of the solid phase extraction tray is 1-5 mm, and the diameter of the section has three standard sizes (25, 47 and 90mm respectively). Wherein, the universal solid phase extraction disc (47 mm diameter, thickness 2.5 mm) can stably realize the sample processing flux of 400-2000mL/min for a large volume of environmental water sample. Under the same conditions, the maximum sample flux recommended for the common EMPORE solid-phase extraction membrane (C18 bonded silica gel or SDB adsorption resin, 47mm diameter) of the same specification is 100mL/min;
(3) The high-flux homogeneous solid phase extraction disk provided by the invention adopts flexible medium-hydrophobic materials, does not need to be activated by a solvent before use, is directly loaded with samples after being manually exhausted and wetted by water, can reduce the solvent consumption in practical operation, simultaneously reduces the pretreatment operation steps and operation time before loading the samples of the solid phase extraction disk, reduces the solvent consumption and is suitable for detecting samples with complex components;
(4) The homogeneous solid phase extraction disc is of a single component structure, the self-supporting framework and the solid phase extraction medium are integrated, complex production and packaging processes are not needed, the disc is cut into standard or custom size according to the requirements after being processed and molded, the disc is suitable for batch production, and compared with EMPORE series products, the disc is low in cost.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The preparation method of the high-flux homogeneous solid phase extraction disc is implemented according to the following steps:
Step 1, weighing polyol, foaming agent, surfactant, catalyst and additive, wherein the addition amount of the foaming agent is 3-30% of the mass of the polyol, the addition amount of the surfactant is 2-3% of the mass of the polyol, the addition amount of the catalyst is 1-2% of the mass of the polyol, and the addition amount of the additive is 1-10% of the mass of the polyol;
Wherein the polyol is polyester, polyether or other alcohols with two or more hydroxyl groups. Specifically, the polymer is any one of polypropylene glycol, trihydroxy polyether, polyoxypropylene glycol, polyester polyol, polycaprolactone polyol or polycarbonate diol. The IOH of the polyol is 15-100 mgKOH/g, and in order to improve the density of the polyurethane soft foam, the polyol with higher IOH value is used to improve the gel rate in the reaction process so that the gel rate is higher than the foaming rate; the higher the functionality, the higher the foam crosslink density of the polyol is, the functionality (f) is 2 to 3; the mol mass of the polyalcohol is 3000-6500 g/mol; the viscosity is 0.2-20 Pa.s.
The foaming agent adopts any one of dichloromethane, trifluoromethane, n-pentane or distilled water. In formulations where the blowing agent is of a certain quality, a lower molar mass blowing agent is selected to produce more foam.
The surfactant is any one of organosilicon surfactant, polyether modified organosilicon surfactant, polysiloxane-polyoxyalkylene ether block copolymer or silicone oil. The surfactant with the lower surface tension is selected to increase the foaming density.
The catalyst adopts any one of triethylenediamine, tin octoate or dibutyltin dilaurate.
The additive is any one of a pore opening agent, a foam stabilizer and a chain extender.
Step 2, mixing the polyol, the foaming agent, the surfactant, the catalyst and the additive which are weighed in the step 1, and stirring for 5-25min at a rotating speed of 1500-2500 r/min to uniformly mix the components, so as to obtain a polyol mixed solution;
Step 3, adding isocyanate into the polyol mixed solution obtained in the step 2, and stirring at a rotating speed of 1000-6000 r/min for 10-60 s to uniformly mix the isocyanate and the polyol mixed solution to obtain a mixture A;
Wherein the isocyanate has two or more isocyanate functional groups, specifically any one of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate or polymethylene diphenyl diisocyanate, and the addition amount of the isocyanate is 100-300% of the mass of the polyol. The addition of the isocyanate mass must correspond to the isocyanate index R, i.e.the molar ratio of-NCO in the isocyanate to-OH in the polyol is from 0.8 to 1.2.
Step 4, continuously stirring the mixture A at a rotating speed of 1000-6000 r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
The solid phase extraction discs prepared by the application are all universal, and the size is as follows: 47mm diameter and 2.5mm thickness. The pore opening agent, the foam stabilizer and the chain extender can be realized by adopting conventional pore opening agents, foam stabilizers and chain extenders.
The process of the invention is further illustrated by the following examples:
Example 1
The preparation method of the high-flux homogeneous solid phase extraction disc is specifically implemented according to the following steps:
Step 1, weighing polypropylene glycol, methylene dichloride, an organosilicon surfactant, triethylenediamine and a pore opening agent, wherein the addition amount of the methylene dichloride is 3% of the mass of the polypropylene glycol, the addition amount of the organosilicon surfactant is 3% of the mass of the polypropylene glycol, the addition amount of the triethylenediamine is 2% of the mass of the polypropylene glycol, and the addition amount of the pore opening agent is 10% of the mass of the polyol;
Step 2, mixing the polypropylene glycol, dichloromethane, the organic silicon surfactant, triethylenediamine and the pore opening agent which are weighed in the step 1, and stirring at a rotating speed of 1500r/min for 25min to uniformly mix the components, so as to obtain a polypropylene glycol mixed solution;
Step 3, adding 300% of toluene diisocyanate by mass of polypropylene glycol into the polypropylene glycol mixed solution obtained in the step 2, and stirring for 60s at a rotating speed of 1000r/min to uniformly mix the mixture to obtain a mixture A;
step 4, continuously stirring the mixture A at a rotating speed of 1000r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
Example 2
The preparation method of the high-flux homogeneous solid phase extraction disc is specifically implemented according to the following steps:
Step 1, weighing trihydroxy polyether, trifluoromethane, polyether modified organic silicon surfactant, tin octoate and foam stabilizer, wherein the addition of the trifluoromethane is 30% of the mass of the trihydroxy polyether, the addition of the polyether modified organic silicon surfactant is 2% of the mass of the trihydroxy polyether, the addition of the tin octoate is 1% of the mass of the trihydroxy polyether, and the addition of the foam stabilizer is 1% of the mass of the trihydroxy polyether;
Step 2, mixing the trihydroxy polyether, the trifluoromethane, the polyether modified organic silicon surfactant, the tin octoate and the foam stabilizer which are weighed in the step1, and stirring for 5min at the rotating speed of 2500r/min to uniformly mix the components, so as to obtain a trihydroxy polyether mixed solution;
Step 3, adding 100% of diphenylmethane diisocyanate by mass of the trihydroxy polyether into the trihydroxy polyether mixed solution obtained in the step 2, and stirring at a rotating speed of 6000r/min for 10s to uniformly mix the mixture to obtain a mixture A;
step 4, continuously stirring the mixture A at a rotating speed of 6000r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
Example 3
The preparation method of the high-flux homogeneous solid phase extraction disc is specifically implemented according to the following steps:
Step 1, weighing polyoxypropylene glycol, n-pentane, polysiloxane-polyoxyalkylene ether block copolymer, dibutyl tin dilaurate and a chain extender, wherein the addition amount of n-pentane is 20% of the mass of the polyoxypropylene glycol, the addition amount of the polysiloxane-polyoxyalkylene ether block copolymer is 2% of the mass of the polyoxypropylene glycol, the addition amount of dibutyl tin dilaurate is 2% of the mass of the polyoxypropylene glycol, and the addition amount of the chain extender is 5% of the mass of the polyoxypropylene glycol;
step 2, mixing the polyoxypropylene glycol, n-pentane, polysiloxane-polyoxyalkylene ether block copolymer, dibutyl tin dilaurate and chain extender which are weighed in the step 1, and stirring at a rotating speed of 2000r/min for 15min to uniformly mix the mixture to obtain a polyoxypropylene glycol mixed solution;
step 3, adding isophorone diisocyanate accounting for 200% of the mass of the polyoxypropylene diol into the polyoxypropylene diol mixed solution obtained in the step 2, and stirring for 30 seconds at the rotating speed of 4000r/min to uniformly mix the components to obtain a mixture A;
Step 4, continuously stirring the mixture A at the rotating speed of 4000r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
Example 4
The preparation method of the high-flux homogeneous solid phase extraction disc is specifically implemented according to the following steps:
Step 1, weighing polyester polyol, distilled water, silicone oil, tin octoate and a foam stabilizer, wherein the addition amount of the distilled water is 25% of the mass of the polyester polyol, the addition amount of the silicone oil is 2.5% of the mass of the polyester polyol, the addition amount of the tin octoate is 1.5% of the mass of the polyester polyol, and the addition amount of the foam stabilizer is 8% of the mass of the polyester polyol;
Step 2, mixing the polyester polyol weighed in the step 1, distilled water, silicone oil, tin octoate and a foam stabilizer, and stirring at a rotation speed of 2300r/min for 10min to uniformly mix the components, thereby obtaining a polyester polyol mixed solution;
Step 3, adding polymethylene diphenyl diisocyanate with the mass of 150% of that of the polyester polyol into the polyester polyol mixed solution obtained in the step 2, and stirring for 25s at a rotating speed of 3000r/min to uniformly mix the polymethylene diphenyl diisocyanate to obtain a mixture A;
step 4, continuously stirring the mixture A at a rotating speed of 3000r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
Example 5
The preparation method of the high-flux homogeneous solid phase extraction disc is specifically implemented according to the following steps:
Step 1, weighing polycaprolactone polyol, trifluoromethane, polyether modified organic silicon surfactant, tin octoate and foam stabilizer, wherein the addition amount of the trifluoromethane is 15% of the mass of the polycaprolactone polyol, the addition amount of the polyether modified organic silicon surfactant is 3% of the mass of the polycaprolactone polyol, the addition amount of the tin octoate is 2% of the mass of the polycaprolactone polyol, and the addition amount of the foam stabilizer is 7% of the mass of the polycaprolactone polyol;
Step 2, mixing the polycaprolactone polyol weighed in the step 1, the trifluoromethane, the polyether modified organic silicon surfactant, the tin octoate and the foam stabilizer, and stirring at a rotating speed of 2000r/min for 15min to uniformly mix the mixture to obtain a polycaprolactone polyol mixed solution;
Step 3, adding 250% of diphenylmethane diisocyanate by mass of the polycaprolactone polyol into the polycaprolactone polyol mixed solution obtained in the step 2, and stirring at the rotating speed of 4000r/min for 25s to uniformly mix the mixture to obtain a mixture A;
Step 4, continuously stirring the mixture A at the rotating speed of 4000r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
Example 6
The preparation method of the high-flux homogeneous solid phase extraction disc is specifically implemented according to the following steps:
Step 1, weighing polycarbonate diol, trifluoromethane, polyether modified organic silicon surfactant, tin octoate and foam stabilizer, wherein the addition of the trifluoromethane is 28% of the mass of the trihydroxy polyether, the addition of the polyether modified organic silicon surfactant is 3% of the mass of the trihydroxy polyether, the addition of the tin octoate is 2% of the mass of the trihydroxy polyether, and the addition of the foam stabilizer is 4% of the mass of the trihydroxy polyether;
step 2, mixing the polycarbonate diol, the trifluoromethane, the polyether modified organic silicon surfactant, the tin octoate and the foam stabilizer which are weighed in the step 1, and stirring for 5min at the rotating speed of 2500r/min to uniformly mix the materials, so as to obtain a polycarbonate diol mixed solution;
Step 3, adding diphenylmethane diisocyanate accounting for 120% of the mass of the polycarbonate diol into the polycarbonate diol mixed solution obtained in the step 2, and stirring at a rotating speed of 6000r/min for 10s to uniformly mix the materials, so as to obtain a mixture A;
step 4, continuously stirring the mixture A at a rotating speed of 6000r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be completely solidified in a natural state, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
Example 7
The preparation method of the high-flux homogeneous solid phase extraction disc is specifically implemented according to the following steps:
Step 1, weighing polycarbonate diol, trifluoromethane, polyether modified organic silicon surfactant, tin octoate and foam stabilizer, wherein the addition amount of the trifluoromethane is 25% of the mass of the trihydroxy polyether, the addition amount of the polyether modified organic silicon surfactant is 3% of the mass of the trihydroxy polyether, the addition amount of the tin octoate is 2% of the mass of the trihydroxy polyether, and the addition amount of the foam stabilizer is 8% of the mass of the trihydroxy polyether;
Step 2, mixing the polycarbonate diol, the trifluoromethane, the polyether modified organic silicon surfactant, the tin octoate and the foam stabilizer which are weighed in the step 1, and stirring at a rotation speed of 2300r/min for 10min to uniformly mix the materials, thereby obtaining a polycarbonate diol mixed solution;
Step3, adding 180% of isocyanate by mass of the polycarbonate diol into the polycarbonate diol mixed solution obtained in the step 2, and stirring for 15s at a rotation speed of 5000r/min to uniformly mix the isocyanate and the polycarbonate diol to obtain a mixture A;
wherein the isocyanate consists of diphenylmethane diisocyanate, isophorone diisocyanate and polymethylene diphenyl diisocyanate, and the mass ratio of the diphenylmethane diisocyanate, the isophorone diisocyanate and the polymethylene diphenyl diisocyanate is as follows: 5:4:1;
step 4, continuously stirring the mixture A at a rotating speed of 5000r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be solidified in a natural state until the mixture A is solidified completely, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
The flux of the homogeneous solid phase extraction discs prepared in examples 1 to 4 above was tested by experiments and the results are shown below:
As can be seen from the above experimental data, the average flux of the homogeneous solid phase extraction disk samples prepared in examples 1 to 4 of the present application is 1013mL/min, and the solid phase extraction disks prepared in examples of the present application are all universal solid phase extraction disks, and the sizes are: the diameter of 47mm and the thickness of 2.5mm can stably realize the sample treatment flux of 400-2000mL/min for a large-volume environmental water sample, and under the same conditions, the maximum sample flux recommended to be used by a common EMPORE solid-phase extraction membrane (C18 bonded silica gel or SDB adsorption resin and 47m m diameter) with the same specification is 100mL/min, so that the sample flux of the homogeneous solid-phase extraction disc prepared by the preparation method is more than 4 times of the sample flux of a EMPORE solid-phase extraction membrane.

Claims (2)

1. The preparation method of the high-flux homogeneous solid phase extraction disc is characterized by comprising the following steps of:
step 1, weighing polyol, a foaming agent, a surfactant, a catalyst and an additive, wherein the addition amount of the foaming agent is 3-30% of the mass of the polyol, the addition amount of the surfactant is 2-3% of the mass of the polyol, the addition amount of the catalyst is 1-2% of the mass of the polyol, and the addition amount of the additive is 1-10% of the mass of the polyol;
the polyol adopts any one of polypropylene glycol, trihydroxy polyether, polyester polyol, polycaprolactone polyol or polycarbonate diol;
step 2, mixing the polyol, the foaming agent, the surfactant, the catalyst and the additive which are weighed in the step 1, and stirring at a rotating speed of 1500-2500 r/min for 5-25min to uniformly mix the components, so as to obtain a polyol mixed solution;
The foaming agent adopts any one of dichloromethane, trifluoromethane, n-pentane or distilled water;
The surfactant adopts an organosilicon surfactant or polyether modified organosilicon surfactant;
the additive is any one of a pore opening agent, a foam stabilizer and a chain extender;
the catalyst adopts any one of triethylenediamine, tin octoate or dibutyltin dilaurate;
step 3, adding isocyanate into the polyol mixed solution obtained in the step 2, and stirring at a rotating speed of 1000-6000 r/min for 10-60 s to uniformly mix the isocyanate and the polyol mixed solution to obtain a mixture A;
The addition amount of isocyanate is 100-300% of the mass of the polyol;
the isocyanate has two or more isocyanate functional groups;
the isocyanate is specifically any one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate or polymethylene diphenyl diisocyanate;
Step 4, continuously stirring the mixture A at a rotating speed of 1000-6000 r/min to enable the mixture A to reach a milky state, pouring the mixture A into a mold to enable the mixture A to be solidified in a natural state until the mixture A is solidified completely, and obtaining the polyurethane soft foam material;
and 5, cutting the polyurethane soft foam material obtained in the step 4 into the standard size and thickness of the solid-phase extraction disc to obtain the high-flux homogeneous solid-phase extraction disc.
2. The method for preparing a high throughput homogeneous solid phase extraction disc according to claim 1, wherein the surfactant is a polysiloxane-polyoxyalkylene ether block copolymer or silicone oil.
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