CN111138570B - Method for treating scum of fluorine-containing dispersion concentrated solution - Google Patents
Method for treating scum of fluorine-containing dispersion concentrated solution Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/18—Monomers containing fluorine
- C08F114/26—Tetrafluoroethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/092—Polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/175—Amines; Quaternary ammonium compounds containing COOH-groups; Esters or salts thereof
Abstract
The invention provides a method for treating scum of fluorine-containing dispersion concentrate, which is characterized in that a first complexing agent and a second complexing agent are added into the fluorine-containing dispersion concentrate; the first complexing agent is one or more of ethylenediamine tetraacetic acid and salts thereof, diethyltriamine pentaacetic acid and salts thereof, citrate, sulfite, triethanolamine, acetylacetone, tartrate and hydroxylamine hydrochloride; the second complexing agent is one or more of oxalic acid, gluconic acid, citric acid and tartaric acid. According to the method provided by the invention, 4-7% of nonionic surfactant is added into the fluorine-containing dispersion liquid in the concentration process, so that the particles are supported in an emulsion system, and the storage stability is excellent; and a specific amount of complexing agent of a specific kind is added at a specific time, so that the obtained fluorine-containing dispersion concentrated solution does not generate scum after being stored for a long time, and each technical index is normal.
Description
Technical Field
The invention belongs to the field of organic high molecular compounds, and particularly relates to a treatment method of a fluorine-containing dispersion liquid.
Background
The fluorine-containing polymer has the characteristics of excellent chemical corrosion resistance, high and low temperature resistance, aging resistance, low friction, non-adhesiveness and the like, so that the fluorine-containing polymer becomes an indispensable special material in the fields of chemical industry, machinery, electricity, construction, medical treatment and the like. Common fluoropolymers include Polytetrafluoroethylene (PTFE), copolymers of Tetrafluoroethylene (TFE) and Hexafluoropropylene (HFP), Perfluoroalkoxy (PFA), ethylene-tetrafluoroethylene (ETFE) copolymers, tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride copolymers, and polyvinylidene fluoride (PVDF), among others.
The fluoropolymer may be prepared by suspension polymerization, emulsion polymerization, solution polymerization, gas phase polymerization, and the like, with emulsion polymerization and suspension polymerization being the most common. In emulsion polymerization, all of the materials are iron-based alloy stainless steel materials due to reaction equipment, concentration equipment, material pipelines, transfer containers and the like, the polymerization process is accompanied by side reaction products and has certain corrosiveness on the equipment materials, and the stainless steel materials generate metal particles due to corrosion, and mainly comprise iron ions, nickel ions, chromium ions, titanium ions and the like. The metal cations are introduced into the production equipment and the package of the fluorine-containing surfactant added into the polymerization system and the nonionic surfactant added after the concentration treatment. Different kinds of metal cations in an alkaline medium, different valence metal ion complexes have different colors, and the color can be displayed on the surface of polymer particles or wrapped in resin particles. The scum in the fluorine-containing dispersion concentrated solution is detected to be iron ions.
Patent US20060135680a1 discloses a process for both reducing the fluorosurfactant content of an aqueous fluoropolymer dispersion containing stable fluorosurfactants containing iron ions and reducing red scum formation. The process comprises contacting the stabilized fluorosurfactant-containing aqueous fluoropolymer dispersion with a strong base anion exchange resin to reduce fluorosurfactant content to a predetermined level. The preferred chelating agent for use in the method is ethylenediaminetetraacetic acid (EDTA) or a salt thereof, in order to minimize the competition of EDTA and fluorosurfactant for ions. This method does not completely avoid scum generation.
Patent CN102161769A discloses a method for preparing an aqueous emulsion of a fluoropolymer, which comprises adding 1 to 15 wt% of a nonionic surfactant and 2 to 20 wt% of an anion exchange resin to a fluoropolymer dispersion having a fluorosurfactant concentration of 500ppm or more, removing the fluorosurfactant and concentrating to obtain a fluoropolymer dispersion having a nonionic surfactant content of 1 to 15 wt%, and adding a mixture of an anionic surfactant, a cationic surfactant, an oxidizing agent and EDTA. The method has complex process, needs ion exchange, anion and cation surfactants and other processes, uses oxydol as an oxidant to convert ferrous ions into ferric ions, and uses EDTA for complexation, and although scum can be reduced, the method has influence on the performance of the emulsion.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for treating scum of fluorine-containing dispersion concentrated solution.
The technical scheme for realizing the purpose of the invention is as follows:
a method for treating scum of fluorine-containing dispersion concentrate comprises adding a first complexing agent and a second complexing agent into the fluorine-containing dispersion concentrate;
the first complexing agent is one or more of ethylenediamine tetraacetic acid and salts thereof, diethyltriamine pentaacetic acid and salts thereof, citrate, sulfite, triethanolamine, acetylacetone, tartrate and hydroxylamine hydrochloride; the second complexing agent is one or more of oxalic acid, gluconic acid, citric acid and tartaric acid.
Wherein the fluorine-containing dispersion concentrated solution is Polytetrafluoroethylene (PTFE) aqueous dispersion prepared by emulsion polymerization; the method of concentrating the dispersion is a vacuum concentration method.
Further, the solid content of the aqueous dispersion liquid obtained by polymerization is 30-35%, and the fluorine-containing dispersion concentrated solution with the solid content of 58-62% is obtained by post-treatment and vacuum concentration.
Wherein the adding amount of the first complexing agent is 30-200 ppm of the weight of PTFE (polytetrafluoroethylene) in the fluorine-containing dispersion concentrated solution; the adding amount of the second complexing agent is 50-300 ppm of the weight of PTFE in the fluorine-containing dispersion concentrated solution.
Preferably, the first complexing agent is EDTA, and the addition amount of the EDTA is 50-150 ppm of the weight of the PTFE in the fluorine-containing dispersion concentrated solution; the second complexing agent is citric acid, and the addition amount of the citric acid is 100-200 ppm of the weight of PTFE in the fluorine-containing dispersion concentrated solution.
The invention provides a preferable technical scheme, which comprises the following steps:
1) adding deionized water, solid paraffin, succinic acid and an ammonium perfluorooctanoate dispersing agent into a reaction kettle, covering a kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding an ammonium persulfate initiator, and controlling the reaction pressure to be 2.0-3.0 Mpa;
2) controlling the polymerization reaction temperature to be 75-90 ℃ to obtain PTFE aqueous dispersion liquid;
3) adding a surfactant into the obtained PTFE aqueous dispersion, and carrying out vacuum concentration to obtain a PTFE concentrated dispersion with a solid content of 60%;
4) sequentially adding 40-150 ppm of disodium ethylene diamine tetraacetate and 90-200 ppm of citric acid based on the weight of PTFE (polytetrafluoroethylene), standing for 5-15 minutes, and adding ammonia water to adjust the pH value to 8.5-9.5.
In the step 1), 20-40 g of solid paraffin, 0.1-0.5 g of succinic acid, 1-2 g of ammonium perfluorooctanoate dispersing agent and 0.005-0.01 g of ammonium persulfate initiator are added into each liter of deionized water.
In the step 3), the surfactant is a nonionic surfactant, and the dosage of the surfactant is 400-450 g per liter of deionized water. The nonionic surfactant added during the concentration is not particularly limited as long as the dispersion can be stabilized during the concentration of the dispersion.
Among them, the step 4) is more preferably: sequentially adding 50ppm of ethylene diamine tetraacetic acid and 100ppm of citric acid based on the weight of PTFE, standing for 10 minutes, and adjusting the pH value to 8.5-9.5 by using ammonia water.
Complexon Fe with disodium ethylenediamine tetraacetate2+The pH value of the environment is more than or equal to 5 and less than 9.6; complexing Fe3+The pH value of the environment is required to be less than or equal to 2, which is difficult to achieve due to the stability and performance of the emulsion. EDTA is usually added in excess. Citric acid over a wide pH rangeIn the enclosure, can be combined with Fe2+、Fe3+Meanwhile, soluble macromolecule ferrous citrate and soluble macromolecule ferric citrate are formed, but the dosage of the macromolecule ferrous citrate and the soluble macromolecule ferric citrate is large, so that the acidity of the emulsion is increased, and the stability and the performance of the emulsion are influenced. Fe, iron citrate, being influenced by light and heat after being made into product3+Gradually reduced to Fe2+At this point, excess EDTA re-complexes it; the ferrous citrate is slowly oxidized by air into reddish brown precipitate after becoming a product, and scum is generated. Therefore, the Fe in the ethylene diamine tetraacetic acid disodium complex emulsion is used2+Fe in citric acid Complex emulsions3+And the single complexing agent cannot completely remove scum in the emulsion and ensure the stability of the performance of the emulsion, and two complexing agents are needed to be matched for use, so that the complexing agent plays a role in complexing iron ions with different prices.
According to the method provided by the invention, 4-7% of nonionic surfactant is added into the fluorine-containing dispersion liquid in the concentration process, so that the particles are supported in an emulsion system, and the storage stability is excellent; and a specific amount of complexing agent of a specific kind is added at a specific time, so that the obtained fluorine-containing dispersion concentrated solution does not generate scum after being stored for a long time, and each technical index is normal.
The method provided by the invention is simple and convenient to operate, and the fluorine-containing dispersion concentrated solution obtained by the method can be stored for a long time without generating scum, and all technical indexes are normal.
Detailed Description
For the sake of understanding, the present invention will be described in detail below with reference to specific examples.
In the examples, unless otherwise specified, all experimental means and equipment are conventional in the art.
Example 1
Adding 28L of deionized water, 1Kg of solid paraffin, 8g of succinic acid and 50g of ammonium perfluorooctanoate dispersing agent into a 50L stainless steel high-pressure reaction kettle which is provided with a jacket and is stirred, covering the kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding 0.2g of ammonium persulfate initiator, and controlling the reaction pressure to be 2.5 MPa. Controlling the polymerization temperature of the reaction to be 75-90 ℃, and stopping the reaction when the feeding amount of the tetrafluoroethylene reaches 20kg to obtain the PTFE aqueous dispersion liquid with the solid content of about 34%.
1.2Kg of nonylphenol polyoxyethylene ether was added to the aqueous dispersion of PTFE, and vacuum concentration was carried out to obtain a concentrated dispersion of PTFE having a solid content of about 60%. 50ppm disodium ethylenediaminetetraacetate and 100ppm citric acid (based on the mass of PTFE) were added in this order, left to stand for 10 minutes (pH at this time was about 5), and ammonia was added to adjust the pH of the concentrated PTFE dispersion to 9.
The obtained PTFE concentrated dispersion liquid is white, after the dispersion liquid is placed for one month, the emulsion is not separated, no red brown scum is generated, and a sample is taken for testing. (see Table 1 for data)
Example 2:
adding 28L of deionized water, 1Kg of solid paraffin, 8g of succinic acid and 50g of ammonium perfluorooctanoate dispersing agent into a 50L stainless steel high-pressure reaction kettle which is provided with a jacket and is stirred, covering the kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding 0.2g of ammonium persulfate initiator, and controlling the reaction pressure to be 2.5 MPa. Controlling the polymerization temperature of the reaction to be 75-90 ℃, and stopping the reaction when the feeding amount of the tetrafluoroethylene reaches 20kg to obtain the PTFE aqueous dispersion liquid with the solid content of about 34%.
1.2Kg of nonylphenol polyoxyethylene ether was added to the aqueous dispersion of PTFE, and vacuum concentration was carried out to obtain a concentrated dispersion of PTFE having a solid content of about 60%. 150ppm disodium ethylene diamine tetraacetate and 200ppm citric acid (based on the mass of PTFE) were added in this order, left to stand for 10 minutes (pH at this time was about 5), and ammonia was added to adjust the pH of the concentrated dispersion of PTFE to 9.
The obtained PTFE concentrated dispersion liquid is white, after the dispersion liquid is placed for one month, the emulsion is not separated, no red brown scum is generated, and a sample is taken for testing. (see Table 1 for data)
Comparative example 1:
adding 28L of deionized water, 1Kg of solid paraffin, 8g of succinic acid and 50g of ammonium perfluorooctanoate dispersing agent into a 50L stainless steel high-pressure reaction kettle which is provided with a jacket and is stirred, covering the kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding 0.2g of ammonium persulfate initiator, and controlling the reaction pressure to be 2.5 MPa. Controlling the polymerization temperature of the reaction to be 75-90 ℃, and stopping the reaction when the feeding amount of the tetrafluoroethylene reaches 20kg to obtain the PTFE aqueous dispersion liquid with the solid content of about 34%.
1.2Kg of nonylphenol polyoxyethylene ether was added to the aqueous dispersion of PTFE to carry out vacuum concentration, thereby obtaining a concentrated dispersion of PTFE having a solid content of about 60%. Adding 300ppm ethylene diamine tetraacetic acid disodium, standing for 10 minutes, and adding ammonia water to adjust the pH value of the PTFE concentrated dispersion liquid to 9.
The obtained PTFE concentrated dispersion liquid is white, after the dispersion liquid is placed for one month, the emulsion is not separated, reddish brown scum is arranged on the upper layer of the emulsion, and a sample is taken for testing. (see Table 1 for data)
Comparative example 2:
adding 28L of deionized water, 1Kg of solid paraffin, 8g of succinic acid and 50g of ammonium perfluorooctanoate dispersing agent into a 50L stainless steel high-pressure reaction kettle which is provided with a jacket and is stirred, covering the kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding 0.2g of ammonium persulfate initiator, and controlling the reaction pressure to be 2.5 MPa. Controlling the polymerization temperature of the reaction to be 75-90 ℃, and stopping the reaction when the feeding amount of the tetrafluoroethylene reaches 20kg to obtain the PTFE aqueous dispersion liquid with the solid content of about 34%.
1.2Kg of nonylphenol polyoxyethylene ether was added to the obtained aqueous dispersion of PTFE to carry out vacuum concentration to obtain a concentrated dispersion of PTFE having a solid content of about 60%, and then ammonia was added to adjust the pH of the concentrated dispersion of PTFE to 9.
The obtained PTFE concentrated dispersion liquid is white, after the dispersion liquid is placed for one month, the emulsion is not separated, reddish brown scum can be seen on the upper layer of the emulsion, and a sample is taken for testing. (see Table 1 for data)
Comparative example 3:
adding 28L of deionized water, 1Kg of solid paraffin, 8g of succinic acid and 50g of ammonium perfluorooctanoate dispersing agent into a 50L stainless steel high-pressure reaction kettle which is provided with a jacket and is stirred, covering the kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding 0.2g of ammonium persulfate initiator, and controlling the reaction pressure to be 2.5 MPa. Controlling the polymerization temperature of the reaction to be 75-90 ℃, and stopping the reaction when the feeding amount of the tetrafluoroethylene reaches 20kg to obtain the PTFE aqueous dispersion liquid with the solid content of about 34%.
1.2Kg of nonylphenol polyoxyethylene ether was added to the aqueous dispersion of PTFE to carry out vacuum concentration, thereby obtaining a concentrated dispersion of PTFE having a solid content of about 60%. 20ppm of disodium ethylene diamine tetraacetate and 30ppm of citric acid were added in this order, and the mixture was allowed to stand for 10 minutes, followed by adjusting the pH of the PTFE concentrated dispersion to 9 with ammonia water.
The obtained PTFE concentrated dispersion liquid is white, after the dispersion liquid is placed for one month, the emulsion is not separated, reddish brown scum can be seen on the upper layer of the emulsion, and a sample is taken for testing. (see Table 1 for data)
Comparative example 4:
adding 28L of deionized water, 1Kg of solid paraffin, 8g of succinic acid and 50g of ammonium perfluorooctanoate dispersing agent into a 50L stainless steel high-pressure reaction kettle which is provided with a jacket and is stirred, covering the kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding 0.2g of ammonium persulfate initiator, and controlling the reaction pressure to be 2.5 MPa. Controlling the polymerization temperature of the reaction to be 75-90 ℃, and stopping the reaction when the feeding amount of the tetrafluoroethylene reaches 20kg to obtain the PTFE aqueous dispersion liquid with the solid content of about 34%.
1.2Kg of nonylphenol polyoxyethylene ether was added to the aqueous dispersion of PTFE to carry out vacuum concentration, thereby obtaining a concentrated dispersion of PTFE having a solid content of about 60%. 500ppm citric acid was added, the mixture was left to stand for 10 minutes, and the pH of the concentrated PTFE dispersion was adjusted to 9 with ammonia water.
The obtained PTFE concentrated dispersion liquid is white, after the dispersion liquid is placed for one month, the emulsion is slightly layered, no red brown scum is generated, and a sample is taken for testing. (see Table 1 for data)
TABLE 1 determination of technical indices of PTFE concentrated dispersions
The experimental result shows that the technical index of the emulsion obtained by the method is normal, has no difference with the technical index of the untreated emulsion, and does not generate scum after being stored for a long time.
The above examples are only for describing the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (4)
1. A method for treating scum of fluorine-containing dispersion concentrate is characterized by comprising the following steps:
1) adding deionized water, solid paraffin, succinic acid and an ammonium perfluorooctanoate dispersing agent into a reaction kettle, covering a kettle cover, vacuumizing to be qualified, introducing a tetrafluoroethylene monomer, adding an ammonium persulfate initiator, and controlling the reaction pressure to be 2.0-3.0 Mpa;
2) controlling the polymerization reaction temperature to be 75-90 ℃ to obtain a polytetrafluoroethylene aqueous dispersion;
3) adding a surfactant into the obtained aqueous dispersion, and carrying out vacuum concentration to obtain a fluorine-containing concentrated dispersion with the solid content of 60%;
4) sequentially adding 40-150 ppm of ethylene diamine tetraacetic acid and 90-200 ppm of citric acid by weight of polytetrafluoroethylene, standing for 5-15 minutes, and adding ammonia water to adjust the pH value to 8.5-9.5.
2. The method of claim 1, wherein in step 1), 20 to 40g of paraffin wax, 0.1 to 0.5g of succinic acid, 1 to 2g of ammonium perfluorooctanoate dispersant, and 0.005 to 0.01g of ammonium persulfate initiator are added per liter of deionized water.
3. The method for treating scum of fluorine-containing dispersion concentrate according to claim 1, wherein in the step 3), the surfactant is a nonionic surfactant, and the amount of the surfactant is 25 to 60g per liter of deionized water.
4. The method for treating scum of fluorine-containing dispersion concentrate according to claim 1, wherein said step 4) is: sequentially adding 50ppm of ethylene diamine tetraacetic acid and 100ppm of citric acid based on the weight of polytetrafluoroethylene, standing for 10 minutes, and then adding ammonia water to adjust the pH value to 8.5-9.5.
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