Preparation process suitable for polyolefin gas exchange membrane

By adding a defoaming agent and scraping off the foam during the preparation of polyolefin gas exchange membranes, the tedious cleaning problem caused by the foam is solved, rapid and efficient mixed liquid preparation is achieved, and production efficiency is improved.

CN120815451APending Publication Date: 2025-10-21ZHONGHENG NEW MATERIAL TECH (SHANDONG) CO LTD
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Patent Information

Application Number
CN202411066698.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2024-04-11
Filing Date
2024-08-05
Publication Date
2025-10-21

AI Technical Summary

Technical Problem

In the existing polyolefin gas exchange membrane preparation process, a large amount of foam is generated when the polyolefin polymer solvent and non-solvent are directly mixed, resulting in a cumbersome cleaning process, reducing production efficiency and making it impossible to achieve fast and efficient mixed liquid preparation.

Method used

During the mixing process, a defoaming agent is added and the upper foam is scraped off by a scraping mechanism. After the casting solution is prepared, spinning, quenching and drying are performed to form a finished exchange membrane.

Benefits of technology

It can directly eliminate foam during mixing, simplify the cleaning process, improve production efficiency, save foam removal time, and make production more efficient.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation process suitable for a polyolefin gas exchange membrane, which specifically comprises the following steps: S1, preparing materials, S2, mixing the materials to prepare a membrane casting solution, S3, spinning and curing, S4, quenching and extracting, and S5, drying: drying membrane filaments extracted in the step S4 through drying equipment, and then forming an exchange membrane finished product through shaping equipment, the invention relates to the technical field of polyolefin gas exchange membrane preparation. According to the preparation process suitable for the polyolefin gas exchange membrane, a large amount of foam in a mixed solution can be eliminated by directly adding a defoaming agent during mixing, and then rapid cleaning is performed through simple scraping, so that the purpose of rapidly and efficiently preparing the mixed solution is well achieved, a large amount of foam removal time is saved, and the production efficiency is improved. The situation that a large amount of foam is generated when all the raw materials are mixed into mixed liquid, and cleaning is conducted through a tedious cleaning method is avoided, the production efficiency is greatly improved, and therefore exchange membrane production of production personnel is greatly facilitated.
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Description

Technical Field

[0001] The invention relates to the technical field of polyolefin gas exchange membrane preparation, in particular to a preparation process suitable for polyolefin gas exchange membranes. Background Art

[0002] Olefin polymers are a general term for thermoplastic resins derived from the polymerization or copolymerization of α-olefins such as ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-octene, and 4-methyl-1-pentene, as well as certain cycloolefins. Due to their abundant raw materials, low cost, ease of processing, and excellent overall performance, they are the most widely produced and widely used polymer materials. Polyethylene and polypropylene are the most important. Key varieties include polyethylene and ethylene-based copolymers such as ethylene-vinyl acetate copolymers and ethylene-acrylic acid or acrylic acid ester copolymers; polypropylene and certain propylene copolymers; poly-1-butene; poly-4-methyl-1-pentene; and cycloolefin polymers. Polyolefins are produced by high-pressure and low-pressure polymerization methods (including solution, slurry, bulk, and vapor phase processes). Polyolefins have low relative density, good chemical and water resistance, and excellent mechanical strength and electrical insulation properties. They can be used in films, pipes, sheets, various molded products, wire and cable, and more. It has a wide range of uses in agriculture, packaging, electronics, electrical appliances, automobiles, machinery, daily necessities, etc. Polyolefin gas exchange membranes play a very important role in chemical production processes.

[0003] In the preparation process of existing polyolefin gas exchange membranes, a solvent for polyolefin polymers and a non-solvent for polyolefin polymers are generally directly mixed and reacted to form a mixed liquid, which is then formed into filaments and membranes. When the raw materials are mixed into the mixed liquid, a large amount of foam is generated, which requires a cumbersome cleaning method, greatly reducing production efficiency. It is not possible to eliminate a large amount of foam in the mixed liquid by directly adding a defoaming agent during mixing, and then quickly clean it by simple scraping. The purpose of preparing the mixed liquid quickly and efficiently cannot be achieved, and a large amount of defoaming time cannot be saved, which brings great inconvenience to the production personnel in the exchange membrane production. Summary of the Invention

[0004] (1) Technical problems solved

[0005] In response to the deficiencies in the prior art, the present invention provides a preparation process suitable for polyolefin gas exchange membranes, which solves the problem that in the existing polyolefin gas exchange membrane preparation process, a solvent for a polyolefin polymer and a non-solvent for a polyolefin polymer are generally directly mixed and reacted to form a mixed liquid, which is then formed into a filament and membrane. When the raw materials are mixed into the mixed liquid, a large amount of foam is generated, which requires a cumbersome cleaning method, greatly reducing production efficiency. It is impossible to eliminate a large amount of foam in the mixed liquid by directly adding a defoaming agent during mixing, and then quickly clean it by simple scraping. Therefore, the purpose of preparing the mixed liquid quickly and efficiently cannot be achieved, and a large amount of foam removal time cannot be saved.

[0006] (2) Technical solution

[0007] To achieve the above objectives, the present invention is implemented through the following technical solutions: A preparation process for a polyolefin gas exchange membrane, specifically comprising the following steps:

[0008] S1. Ingredients: Weigh the required weight portions of dioctyl adipate, triacetin, isopropyl myristate, diethyl phthalate, diphenyl ether, N,N-bis(2-hydroxyethyl) tallowamine, dibenzyl ether, natural oil organic solvent, defoamer, and film-forming agent using a batching device, and store the weighed raw materials in a storage device for later use;

[0009] S2. Mixing to prepare a casting solution: pouring the dioctyl adipate, triacetin, isopropyl myristate, diethyl phthalate, diphenyl ether, N,N-bis(2-hydroxyethyl) tallow amine, dibenzyl ether, and natural oil organic solvent weighed in step S1 into a mixing reaction device in sequence, mixing for 1-2 hours at a temperature above the critical delamination temperature, then pouring the defoaming agent and film-forming agent weighed in step S1 into the mixing reaction device in sequence, starting the mixing and stirring device at a speed of 300-500 r / min, and stirring for 20-30 minutes. A small amount of foam will be generated on the upper layer of the mixed solution, and then the upper layer foam is scraped off by a scraping mechanism, and then the lower layer of the mixed solution is transferred out of the mixing reaction device to obtain a casting solution;

[0010] S3, spinning and solidification: the casting solution obtained in step S2 is extruded through a spinning device to form membrane filaments, and then the membrane filaments are immersed in a cooling liquid for phase separation and solidification;

[0011] S4, quenching and extraction: placing the membrane filaments solidified in step S2 into a quenching furnace for quenching treatment to pre-shape the membrane filaments and eliminate their internal stress, and then immersing the quenched membrane filaments in an extraction solution for extraction;

[0012] S5, drying: the membrane fibers extracted in step S4 are dried by a drying device, and then passed through a shaping device to form a finished exchange membrane.

[0013] Preferably, the raw materials weighed in step S1 include, by weight, 5-10 parts of dioctyl adipate, 5-10 parts of triacetin, 5-10 parts of isopropyl myristate, 5-10 parts of diethyl phthalate, 5-10 parts of diphenyl ether, 5-10 parts of N,N-bis(2-hydroxyethyl)tallowamine, 5-10 parts of dibenzyl ether, 10-20 parts of natural oil organic solvent, 3-5 parts of defoaming agent and 3-5 parts of film-forming agent.

[0014] Preferably, the raw materials weighed in step S1 include, by weight, 7 parts of dioctyl adipate, 7 parts of triacetin, 7 parts of isopropyl myristate, 7 parts of diethyl phthalate, 7 parts of diphenyl ether, 7 parts of N,N-bis(2-hydroxyethyl)tallowamine, 7 parts of dibenzyl ether, 15 parts of natural oil organic solvent, 4 parts of defoaming agent and 4 parts of film-forming agent.

[0015] Preferably, the raw materials weighed in step S1 include, by weight, 5 parts of dioctyl adipate, 5 parts of triacetin, 5 parts of isopropyl myristate, 5 parts of diethyl phthalate, 5 parts of diphenyl ether, 5 parts of N,N-bis(2-hydroxyethyl)tallowamine, 5 parts of dibenzyl ether, 10 parts of natural oil organic solvent, 3 parts of defoaming agent and 3 parts of film-forming agent.

[0016] Preferably, the raw materials weighed in step S1 include, by weight, 10 parts of dioctyl adipate, 10 parts of triacetin, 10 parts of isopropyl myristate, 10 parts of diethyl phthalate, 10 parts of diphenyl ether, 10 parts of N,N-bis(2-hydroxyethyl)tallowamine, 10 parts of dibenzyl ether, 20 parts of natural oil organic solvent, 5 parts of defoaming agent and 5 parts of film-forming agent.

[0017] Preferably, the natural oil organic solvent in step S1 is one of castor oil, soybean oil or rapeseed oil.

[0018] Preferably, the viscosity of the casting solution prepared in step S2 is 2000-3000 CPS.

[0019] Preferably, the scraping mechanism in step S2 includes a driving motor, a scraping rod, and an electric telescopic rod for controlling the lifting of the scraping rod, which are arranged on the reaction equipment.

[0020] (3) Beneficial effects

[0021] The present invention provides a preparation process for polyolefin gas exchange membranes. Compared with the prior art, the present invention has the following advantages: the preparation process for polyolefin gas exchange membranes specifically comprises the following steps: S1, batching, S2, mixing to prepare a casting solution, S3, spinning and solidifying: extruding the casting solution obtained in step S2 through a spinning device to form membrane filaments, and then immersing the membrane filaments in a cooling liquid for phase separation and solidification; S4, quenching and extracting: placing the membrane filaments solidified in step S2 into a quenching furnace for quenching treatment, pre-forming the membrane filaments and eliminating their internal stress, and then immersing the quenched membrane filaments in an extraction liquid for extraction; S5, drying: The membrane fibers extracted in step S4 are dried by a drying device and then formed into a finished exchange membrane product by a shaping device. The foam in the mixed liquid can be eliminated in large quantities by directly adding a defoaming agent during mixing, and then quickly cleaned by simple scraping, which well achieves the purpose of preparing the mixed liquid quickly and efficiently, saves a lot of foam removal time, and well avoids the generation of a large amount of foam when mixing the raw materials into a mixed liquid, and the occurrence of cumbersome cleaning methods for cleaning, which greatly improves production efficiency and greatly facilitates the exchange membrane production of production personnel. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is the process flow chart of the present invention. DETAILED DESCRIPTION

[0023] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0024] See also Figure 1 The present invention provides three technical solutions: a preparation process for a polyolefin gas exchange membrane, specifically including the following embodiments:

[0025] Example 1

[0026] S1. Ingredients: Weigh the required weight portions of 7 parts of dioctyl adipate, 7 parts of triacetin, 7 parts of isopropyl myristate, 7 parts of diethyl phthalate, 7 parts of diphenyl ether, 7 parts of N,N-bis(2-hydroxyethyl) tallowamine, 7 parts of dibenzyl ether, 15 parts of natural oil organic solvent, 4 parts of defoaming agent and 4 parts of film-forming agent respectively through a batching device, and store the weighed raw materials in a storage device for use. The natural oil organic solvent is castor oil;

[0027] S2. Mixing to prepare a casting solution: pouring the dioctyl adipate, triacetin, isopropyl myristate, diethyl phthalate, diphenyl ether, N,N-bis(2-hydroxyethyl) tallow amine, dibenzyl ether and natural oil organic solvent weighed in step S1 into a mixing reaction device in sequence, mixing for 1.5 hours under a condition higher than the critical delamination temperature, then pouring the defoamer and film-forming agent weighed in step S1 into the mixing reaction device in sequence, starting the mixing and stirring device and mixing and stirring at a speed of 400 r / min for 25 minutes, a small amount of foam will be generated on the upper layer of the mixed solution, and then the upper foam will be scraped out by a scraping mechanism, and then the mixed solution in the lower layer will be transferred out from the mixing reaction device to obtain a casting solution, the viscosity of the casting solution is 2500 CPS, and the scraping mechanism includes a drive motor, a scraping rod and an electric telescopic rod for controlling the lifting of the scraping rod, which are arranged on the reaction device;

[0028] S3, spinning and solidification: the casting solution obtained in step S2 is extruded through a spinning device to form membrane filaments, and then the membrane filaments are immersed in a cooling liquid for phase separation and solidification;

[0029] S4, quenching and extraction: placing the membrane filaments solidified in step S2 into a quenching furnace for quenching treatment to pre-shape the membrane filaments and eliminate their internal stress, and then immersing the quenched membrane filaments in an extraction solution for extraction;

[0030] S5, drying: the membrane fibers extracted in step S4 are dried by a drying device, and then passed through a shaping device to form a finished exchange membrane.

[0031] Example 2

[0032] S1. Ingredients: Weigh the required weight portions of 5 parts of dioctyl adipate, 5 parts of triacetin, 5 parts of isopropyl myristate, 5 parts of diethyl phthalate, 5 parts of diphenyl ether, 5 parts of N,N-bis(2-hydroxyethyl) tallowamine, 5 parts of dibenzyl ether, 10 parts of natural oil organic solvent, 3 parts of defoaming agent and 3 parts of film-forming agent respectively through a batching device, and store the weighed raw materials in a storage device for use. The natural oil organic solvent is soybean oil;

[0033] S2. Mixing to prepare a casting solution: pouring the dioctyl adipate, triacetin, isopropyl myristate, diethyl phthalate, diphenyl ether, N,N-bis(2-hydroxyethyl) tallow amine, dibenzyl ether and natural oil organic solvent weighed in step S1 into a mixing reaction device in sequence, mixing for 1 hour under a condition above the critical delamination temperature, then pouring the defoamer and film-forming agent weighed in step S1 into the mixing reaction device in sequence, starting the mixing and stirring device at a speed of 300 r / min and stirring for 20 minutes, a small amount of foam will be generated on the upper layer of the mixed solution, and then scraping the upper foam out by a scraping mechanism, and then transferring the lower layer of the mixed solution from the mixing reaction device to obtain a casting solution, the viscosity of the casting solution is 2000 CPS, and the scraping mechanism includes a drive motor, a scraping rod and an electric telescopic rod for controlling the lifting of the scraping rod, which are arranged on the reaction device;

[0034] S3, spinning and solidification: the casting solution obtained in step S2 is extruded through a spinning device to form membrane filaments, and then the membrane filaments are immersed in a cooling liquid for phase separation and solidification;

[0035] S4, quenching and extraction: placing the membrane filaments solidified in step S2 into a quenching furnace for quenching treatment to pre-shape the membrane filaments and eliminate their internal stress, and then immersing the quenched membrane filaments in an extraction solution for extraction;

[0036] S5, drying: the membrane fibers extracted in step S4 are dried by a drying device, and then passed through a shaping device to form a finished exchange membrane.

[0037] Example 3

[0038] S1. Ingredients: 10 parts of dioctyl adipate, 10 parts of triacetin, 10 parts of isopropyl myristate, 10 parts of diethyl phthalate, 10 parts of diphenyl ether, 10 parts of N,N-bis(2-hydroxyethyl) tallowamine, 10 parts of dibenzyl ether, 20 parts of natural oil organic solvent, 5 parts of defoaming agent and 5 parts of film-forming agent are weighed respectively by a batching device in the required weight portions, and the weighed raw materials are stored in a storage device for standby use. The natural oil organic solvent is rapeseed oil;

[0039] S2. Mixing to prepare a casting solution: pouring the dioctyl adipate, triacetin, isopropyl myristate, diethyl phthalate, diphenyl ether, N,N-bis(2-hydroxyethyl) tallow amine, dibenzyl ether and natural oil organic solvent weighed in step S1 into a mixing reaction device in sequence, and mixing for 2 hours under a condition higher than the critical delamination temperature, then pouring the defoamer and film-forming agent weighed in step S1 into the mixing reaction device in sequence, starting the mixing and stirring device and mixing and stirring at a speed of 500 r / min for 30 minutes, a small amount of foam will be generated on the upper layer of the mixed solution, and then scraping the upper foam out by a scraping mechanism, and then transferring the lower layer of the mixed solution from the mixing reaction device to obtain a casting solution, the viscosity of the casting solution is 3000 CPS, and the scraping mechanism includes a drive motor, a scraping rod and an electric telescopic rod for controlling the lifting of the scraping rod, which are arranged on the reaction device;

[0040] S3, spinning and solidification: the casting solution obtained in step S2 is extruded through a spinning device to form membrane filaments, and then the membrane filaments are immersed in a cooling liquid for phase separation and solidification;

[0041] S4, quenching and extraction: placing the membrane filaments solidified in step S2 into a quenching furnace for quenching treatment to pre-shape the membrane filaments and eliminate their internal stress, and then immersing the quenched membrane filaments in an extraction solution for extraction;

[0042] S5, drying: the membrane fibers extracted in step S4 are dried by a drying device, and then passed through a shaping device to form a finished exchange membrane.

[0043] In summary, the present invention can eliminate a large amount of foam in the mixed liquid by directly adding a defoaming agent during mixing, and then quickly clean it up by simple scraping, thereby achieving the purpose of preparing the mixed liquid quickly and efficiently, saving a lot of foam removal time, and avoiding the generation of a large amount of foam when mixing the raw materials into a mixed liquid, and the occurrence of cumbersome cleaning methods for cleaning, which greatly improves production efficiency and greatly facilitates the exchange membrane production of production personnel.

[0044] Meanwhile, the contents not described in detail in this specification belong to the prior art known to those skilled in the art.

[0045] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0046] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A process for preparing a polyolefin gas exchange membrane, characterized in that: The specific steps include: S1. Ingredients: Weigh the required weight portions of dioctyl adipate, triacetin, isopropyl myristate, diethyl phthalate, diphenyl ether, N,N-bis(2-hydroxyethyl) tallowamine, dibenzyl ether, natural oil organic solvent, defoamer, and film-forming agent using a batching device, and store the weighed raw materials in a storage device for later use; S2. Mixing to prepare a casting solution: pouring the dioctyl adipate, triacetin, isopropyl myristate, diethyl phthalate, diphenyl ether, N,N-bis(2-hydroxyethyl) tallow amine, dibenzyl ether, and natural oil organic solvent weighed in step S1 into a mixing reaction device in sequence, mixing for 1-2 hours at a temperature above the critical delamination temperature, then pouring the defoaming agent and film-forming agent weighed in step S1 into the mixing reaction device in sequence, starting the mixing and stirring device at a speed of 300-500 r / min, and stirring for 20-30 minutes. A small amount of foam will be generated on the upper layer of the mixed solution, and then the upper layer foam is scraped off by a scraping mechanism, and then the lower layer of the mixed solution is transferred out of the mixing reaction device to obtain a casting solution; S3, spinning and solidification: the casting solution obtained in step S2 is extruded through a spinning device to form membrane filaments, and then the membrane filaments are immersed in a cooling liquid for phase separation and solidification; S4, quenching and extraction: placing the membrane filaments solidified in step S2 into a quenching furnace for quenching treatment to pre-shape the membrane filaments and eliminate their internal stress, and then immersing the quenched membrane filaments in an extraction solution for extraction; S5, drying: the membrane fibers extracted in step S4 are dried by a drying device, and then passed through a shaping device to form a finished exchange membrane.

2. The process for preparing a polyolefin gas exchange membrane according to claim 1, wherein: The raw materials weighed in step S1 include, by weight, 5-10 parts of dioctyl adipate, 5-10 parts of triacetin, 5-10 parts of isopropyl myristate, 5-10 parts of diethyl phthalate, 5-10 parts of diphenyl ether, 5-10 parts of N,N-bis(2-hydroxyethyl)tallowamine, 5-10 parts of dibenzyl ether, 10-20 parts of natural oil organic solvent, 3-5 parts of defoaming agent, and 3-5 parts of film-forming agent.

3. The process for preparing a polyolefin gas exchange membrane according to claim 1, wherein: The raw materials weighed in step S1 include, by weight, 7 parts of dioctyl adipate, 7 parts of triacetin, 7 parts of isopropyl myristate, 7 parts of diethyl phthalate, 7 parts of diphenyl ether, 7 parts of N,N-bis(2-hydroxyethyl)tallowamine, 7 parts of dibenzyl ether, 15 parts of natural oil organic solvent, 4 parts of defoaming agent, and 4 parts of film-forming agent.

4. The process for preparing a polyolefin gas exchange membrane according to claim 1, wherein: The raw materials weighed in step S1 include, by weight, 5 parts of dioctyl adipate, 5 parts of triacetin, 5 parts of isopropyl myristate, 5 parts of diethyl phthalate, 5 parts of diphenyl ether, 5 parts of N,N-bis(2-hydroxyethyl)tallowamine, 5 parts of dibenzyl ether, 10 parts of natural oil organic solvent, 3 parts of defoaming agent, and 3 parts of film-forming agent.

5. The process for preparing a polyolefin gas exchange membrane according to claim 1, wherein: The raw materials weighed in step S1 include, by weight, 10 parts of dioctyl adipate, 10 parts of triacetin, 10 parts of isopropyl myristate, 10 parts of diethyl phthalate, 10 parts of diphenyl ether, 10 parts of N,N-bis(2-hydroxyethyl) tallowamine, 10 parts of dibenzyl ether, 20 parts of natural oil organic solvent, 5 parts of defoaming agent, and 5 parts of film-forming agent.

6. A process for preparing a polyolefin gas exchange membrane according to any one of claims 1 to 5, characterized in that: The natural oil organic solvent in step S1 is one of castor oil, soybean oil or rapeseed oil.

7. The process for preparing a polyolefin gas exchange membrane according to claim 1, wherein: The viscosity of the casting solution prepared in step S2 is 2000-3000 CPS.

8. The process for preparing a polyolefin gas exchange membrane according to claim 1, wherein: The scraping mechanism in step S2 includes a driving motor, a scraping rod, and an electric telescopic rod for controlling the lifting of the scraping rod, which are arranged on the reaction equipment.