CN112647306B - Solid-liquid mixed type foam stabilizer and preparation method thereof - Google Patents
Solid-liquid mixed type foam stabilizer and preparation method thereof Download PDFInfo
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- CN112647306B CN112647306B CN202011244351.9A CN202011244351A CN112647306B CN 112647306 B CN112647306 B CN 112647306B CN 202011244351 A CN202011244351 A CN 202011244351A CN 112647306 B CN112647306 B CN 112647306B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
- D06N3/005—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers obtained by blowing or swelling agent
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
- D06N3/0047—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers obtained by incorporating air, i.e. froth
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0061—Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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- D06N2209/00—Properties of the materials
- D06N2209/10—Properties of the materials having mechanical properties
- D06N2209/103—Resistant to mechanical forces, e.g. shock, impact, puncture, flexion, shear, compression, tear
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- D06N2211/00—Specially adapted uses
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Abstract
The invention discloses a solid-liquid mixed type foam stabilizer and a preparation method thereof. The solid-liquid mixed type foam stabilizer comprises emulsion and solid particles, wherein the emulsion is potassium stearate emulsion and/or sodium stearate emulsion, and the solid particles are calcium carbonate particles with stearic acid molecules chemically grafted on the surface; the foam stabilizer is prepared by reacting raw materials containing stearic acid, sodium hydroxide and/or potassium hydroxide and calcium carbonate particles. The preparation method comprises the following steps: adding an organic solvent, stearic acid and calcium carbonate particles into a reaction kettle, adjusting the temperature to 40-65 ℃, and mixing and stirring; continuously dripping alkaline water solution, and reacting for 2-4 hours after finishing dripping; after the reaction is finished, sufficient water is supplemented into the reaction kettle; shearing and emulsifying at high speed to obtain final product. The solid-liquid mixed type foam stabilizer provided by the invention overcomes the problem of poor foam stabilizing performance of the traditional sodium soap and potassium soap emulsion, and the foam stabilizing performance of the obtained mixed type foam stabilizer is remarkably improved and is better than that of the traditional ammonium stearate emulsion.
Description
Technical Field
The invention relates to a foam stabilizer and a preparation method thereof, in particular to a solid-liquid mixed type foam stabilizer and a preparation method thereof, and belongs to the technical field of chemical assistants.
Background
The water-based polymer foam coating is coated on the surface of the fabric or the cloth base, and is widely applied to the production process of PU synthetic leather and shading cloth. The coating layer has the performances of flame retardance, stain resistance, shading and the like, and enables the fabric or the fabric base to have unique style, hand feeling and appearance. The production process of the water-based polymer foaming coating comprises the steps of adding a foaming agent (generally a surfactant) into finishing working solution, mixing the foaming agent with air by using foaming equipment to form foam slurry, and uniformly applying foam to the surface of a fabric or a fabric substrate by using a foam applicator.
Foam stabilizers are often added during the preparation of foamed coatings because foams are unstable systems that spontaneously aggregate and disproportionate. According to literature reports, the foam stabilizers commonly used at present can be divided into surfactants, proteins, polymers and the like. In the production practice of the water-based polymer foaming coating, the most widely used foam stabilizer is ammonium stearate emulsion, and compared with the problems of high viscosity, easy agglomeration, easy caking and the like in the preparation process of potassium (sodium) stearate emulsions of the same type, the ammonium stearate emulsion has the advantages of simple preparation process and low price; moreover, the foam stabilizing performance of the ammonium stearate emulsion is better than that of the potassium (sodium) stearate emulsion. However, the ammonium stearate emulsion requires a large amount of ammonia water during its production and preparation, so that the final product has a strong pungent odor. And the saponification rate of the ammonium stearate emulsion prepared by the prior art is low, so that the content of active substance ammonium stearate in the product is low, and the ammonium stearate emulsion is large in dosage when used as a foam stabilizer.
Calcium carbonate (CaCO) 3 ) Is an important inorganic chemical product, has the advantages of wide raw material source, low price and the like, and can be widely applied to industries such as rubber, plastics, paint, papermaking ink and the like as a filler. It can greatly raise heat-resisting and wear-resisting properties of product, and can reduce cost of product. The applicant has also used solid calcium carbonate particles as foam stabilizers alone in the prior application patent, and the pore size of the foamed coating is obviously smaller after the foamed coating is formed, but the pore dispersibility is equivalent to that of the traditional ammonium stearate emulsion and is not improved obviously.
Based on this, the applicant further studied and formed the technology of the present invention.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems of the existing ammonium stearate emulsion foam stabilizer, the invention provides a solid-liquid mixed type foam stabilizer and a preparation method of the mixed type foam stabilizer.
The technical scheme is as follows: the solid-liquid mixed type foam stabilizer comprises emulsion and solid particles, wherein the emulsion is sodium stearate emulsion and/or potassium stearate emulsion, and the solid particles are calcium carbonate particles with stearic acid molecules chemically grafted on the surface; the solid-liquid mixed type foam stabilizer is prepared by reacting raw materials containing stearic acid, sodium hydroxide and/or potassium hydroxide and calcium carbonate particles.
Among them, the particle size of the calcium carbonate particles is preferably in the range of 0.5 to 5 μm. Preferably, the mass ratio of calcium carbonate to stearic acid in the raw materials is 1:2-2:1, and the molar ratio of sodium hydroxide and/or potassium hydroxide to stearic acid is 1:1-2:1.
The preparation method of the solid-liquid mixed type foam stabilizer comprises the following steps:
(1) Adding an organic solvent, stearic acid and calcium carbonate particles into a reaction kettle, adjusting the temperature to 40-65 ℃, and mixing and stirring;
(2) Dropwise adding an alkaline water solution into the reaction kettle, and reacting for 2-4 hours after the dropwise adding of the alkaline water solution is finished;
(3) After the reaction is finished, supplementing water into the reaction kettle according to the condition that the addition amount of stearic acid accounts for 10-20% of the total amount of the raw materials;
(4) And (4) shearing and emulsifying the product obtained in the step (3) at a high speed to obtain a final product.
In the preparation method, the total mass of the raw materials of the organic solvent, the stearic acid, the calcium carbonate particles, the aqueous alkali solution and the water is 100 percent, the addition amount of the stearic acid is 10 to 20 percent, the mass ratio of the organic solvent to the stearic acid is 1:2 to 2:1, the mass ratio of the calcium carbonate particles to the stearic acid is 1:2 to 2:1, the molar ratio of the total molar amount of hydroxide radicals in the aqueous alkali solution to the stearic acid is 1:1 to 2:1, and the balance is water.
Optionally, the organic solvent in step (1) is at least one of propylene glycol and ethylene glycol. In the step (2), the aqueous alkali solution may be at least one of potassium hydroxide and sodium hydroxide.
In the step (4), the speed of shearing emulsification is preferably 10000-20000 r/min, and the emulsification time is preferably 30-60 min.
The invention principle is as follows: the solid-liquid mixed type foam stabilizer takes stearic acid, calcium carbonate, alkaline water and the like as raw materials, and during preparation, the stearic acid is dissolved by an organic solvent, then the stearic acid is deprotonated in the presence of the alkaline water and is adsorbed on the surface of the calcium carbonate in the form of ionic bonds, and then the stearic acid reacts with the calcium carbonate to generate calcium stearate precipitates, so that calcium carbonate particles with stearic acid molecules chemically grafted on the surface are formed (the stearic acid and the calcium carbonate are difficult to react under the normal condition); meanwhile, a surfactant potassium stearate/sodium soap is generated in the system, and the soap surfactant and the calcium carbonate particles with amphipathy after chemical grafting can be adsorbed on a gas-liquid interface at the same time, so that an interface film is more compact, coalescence and disproportionation among bubbles are prevented, and the foam stability is greatly improved.
Has the advantages that: compared with the prior art, the invention has the advantages that: (1) The main components of the solid-liquid mixed type foam stabilizer are sodium stearate/potassium stearate emulsion and calcium carbonate particles with stearic acid grafted on the surface, the problem of poor foam stabilizing performance of the traditional sodium soap and potassium soap is solved after solid-liquid mixing, the foam stabilizing performance of the obtained mixed type foam stabilizer is remarkably improved, and the mixed type foam stabilizer is better than the traditional ammonium stearate; (2) Compared with the traditional ammonium stearate emulsion, the solid-liquid mixed type foam stabilizer is convenient to prepare, and the potassium hydroxide and/or the sodium hydroxide are/is used for replacing ammonia water, so that the pungent smell of the product is eliminated, the working environment is improved, and the solid-liquid mixed type foam stabilizer is more green and environment-friendly; moreover, the saponification rate is obviously improved, the content of active substances is increased, and the dosage of the water-based polymer foaming coating prepared by the water-based polymer foaming coating serving as a foam stabilizer is greatly reduced; (3) The solid-liquid mixed type foam stabilizer provided by the invention introduces solid particles into the traditional emulsion type foam stabilizer, so that when the solid-liquid mixed type foam stabilizer is used in a water-based polymer foaming system, the production cost of a coating can be reduced, and the mechanical strength of the coating can be obviously improved.
Drawings
Fig. 1 is a tensile stress curve of a polyurethane foam coating prepared by using the foam stabilizer and ammonium stearate emulsion of examples 1-4, wherein curve a corresponds to example 2, curve b corresponds to example 1, curve c corresponds to example 3, curve d corresponds to example 4, and curve e corresponds to ammonium stearate emulsion.
Detailed Description
The technical solution of the present invention is further explained below.
The solid-liquid mixed type foam stabilizer comprises emulsion and solid particles, wherein the emulsion is sodium stearate emulsion and/or potassium stearate emulsion, and the solid particles are calcium carbonate particles with stearic acid molecules chemically grafted on the surface. After solid and liquid are mixed, the problem of poor foam stabilizing performance of the traditional sodium soap and potassium soap is solved, the foam stabilizing performance of the obtained mixed type foam stabilizer is obviously improved, and the mixed type foam stabilizer is better than the traditional ammonium stearate.
Example 1
1) Weighing 20 parts of propylene glycol, 20 parts of stearic acid and 10 parts of calcium carbonate (with the particle size of 2 microns) particles in a reaction kettle, controlling the temperature to be 50 ℃, and mixing and stirring to prepare suspension;
2) Then 20 parts of potassium hydroxide solution (n) with the mass fraction of 20 percent are added dropwise Potassium hydroxide :n Stearic acid = 1:1), stirring is continued for 3 hours at 50 ℃;
3) After the reaction is finished, continuously supplementing water into the reaction kettle until the total mass of the product is 100 parts, and mixing and stirring for 10 minutes;
4) And emulsifying the product (the shearing rate is 10000r/min, and the emulsifying time is 60 min) to obtain the final product.
Example 2
1) Weighing 10 parts of ethylene glycol, 10 parts of stearic acid and 20 parts of calcium carbonate (with the particle size of 0.5 micron) particles in a reaction kettle, controlling the temperature to be 40 ℃, and mixing and stirring to prepare suspension;
2) Then 20 parts of 10 percent potassium hydroxide solution (n) by mass fraction Potassium hydroxide :n Stearic acid = 1:1), stirring at 40 ℃ for 4 hours;
3) After the reaction is finished, continuously supplementing water into the reaction kettle until the total mass of the product is 100 parts, and mixing and stirring for 10 minutes;
4) The product is emulsified (shear rate 15000r/min, emulsifying time 45 min) to obtain the final product.
Example 3
1) Weighing 20 parts of propylene glycol, 10 parts of stearic acid and 20 parts of calcium carbonate (with the particle size of 5 microns) particles in a reaction kettle, controlling the temperature to be 65 ℃, and mixing and stirring to prepare suspension;
2) Then 20 parts of potassium hydroxide solution (n) with the mass fraction of 20 percent are added Potassium hydroxide :n Stearic acid = 2:1), stirring is continued for 2 hours at 65 ℃;
3) After the reaction is finished, continuously supplementing water into the reaction kettle until the total mass of the product is 100 parts, and mixing and stirring for 10 minutes;
4) The product is emulsified (shear rate 20000r/min, emulsification time 30 min) to obtain the final product.
Example 4
1) Weighing 10 parts of ethylene glycol, 20 parts of stearic acid and 15 parts of calcium carbonate (with the particle size of 2 microns) particles in a reaction kettle, controlling the temperature to be 50 ℃, and mixing and stirring to prepare suspension;
2) Then 20 parts of sodium hydroxide solution (n) with the mass fraction of 14 percent are added Sodium hydroxide (NaOH) :n Stearic acid = 1:1), stirring at 50 ℃ is continued for 2 hours;
3) After the reaction is finished, continuously supplementing water into the reaction kettle until the total mass of the product is 100 parts, and mixing and stirring for 10 minutes;
4) And emulsifying the product (the shearing rate is 10000r/min, and the emulsifying time is 60 min) to obtain the final product.
The calcium carbonate particle foam stabilizer prepared in examples 1 to 4 and the comparative ammonium stearate foam stabilizer (solid content: 30%) were used as foam stabilizers for aqueous polymer emulsion foam coatings. The concrete dosage of the mixed foam stabilizer and the ammonium stearate foam stabilizer is as shown in the following table 1, and the water-based polymer emulsion foaming coating is prepared according to the following steps:
s1, 100g of polyurethane emulsion, 10-20g of foam stabilizer and 1g of thickener are uniformly mixed.
And S2, rapidly stirring by using an electric foaming machine to prepare foaming slurry.
And S3, coating the foaming slurry on release paper by using a film scraper, and drying in a drying oven at 100 ℃ after coating to obtain the water-based polymer emulsion foaming coating.
Structural characterization of the high-molecular foaming coating: the pore size and the pore size distribution of the foam coatings prepared by using the foam stabilizers are observed by an optical microscope and a scanning electron microscope, and the test results are shown in table 1.
Testing the mechanical property of the polymer foaming coating: the mechanical properties of the foamed coatings prepared in examples 1-4 and comparative examples of ammonium stearate foam stabilizer were tested according to the determination of tensile strength and elongation in physical and mechanical tests of leather (QB/T2710-2018), and the test results are shown in FIG. 1.
Testing parameters of tactile properties of the polymer foam coating: the tactile properties of the foamed coatings were tested and the results are shown in table 1.
TABLE 1 Structure and Performance test results of aqueous polymer foam coatings prepared with different foam stabilizers
As can be seen from table 1, the coatings prepared by the solid-liquid mixed type foam stabilizers prepared in examples 1 to 4 of the present invention have smaller pore size and lower PDI value compared with the coating prepared by the comparative ammonium stearate emulsion, which indicates that the pore distribution of the foamed coating is more uniform, i.e., the foam stabilizing performance of the solid-liquid mixed type foam stabilizer of the present invention is better than that of the conventional ammonium stearate foam stabilizer.
The elasticity and softness of the foaming coating prepared based on different foam stabilizers are tested, and the result shows that the foaming coating prepared by the solid-liquid mixed type foam stabilizer has active hand feeling and good softness.
As shown in fig. 1, based on the mechanical property test of the polymer foam coatings prepared by the ammonium stearate emulsion foam stabilizers in examples 1 to 4 and the comparative example, it can be seen that the tensile stress and tensile strain of the coatings prepared by the solid-liquid mixed foam stabilizers prepared in examples 1 to 4 are significantly improved compared with the coatings prepared by the comparative example ammonium stearate emulsion, which indicates that the strength and toughness of the aqueous polymer foam coatings can be significantly improved by the solid-liquid mixed foam stabilizers.
Claims (6)
1. The solid-liquid mixed type foam stabilizer is characterized by comprising an emulsion and solid particles, wherein the emulsion is a sodium stearate emulsion and/or a potassium stearate emulsion, and the solid particles are calcium carbonate particles with stearic acid molecules chemically grafted on the surface; the solid-liquid mixed type foam stabilizer is prepared by reacting raw materials containing stearic acid, sodium hydroxide and/or potassium hydroxide and calcium carbonate particles;
the particle size of the calcium carbonate particles is 0.5 to 5 mu m;
the mass ratio of the calcium carbonate particles to stearic acid is 1 to 2;
the molar ratio of the sodium hydroxide and/or the potassium hydroxide to the stearic acid is 1 to 1.
2. The preparation method of the solid-liquid mixed foam stabilizer of claim 1, which is characterized by comprising the following steps:
(1) Adding an organic solvent, stearic acid and calcium carbonate particles into a reaction kettle, adjusting the temperature to 40-65 ℃, mixing and stirring;
(2) Dropwise adding an aqueous alkali solution into the reaction kettle, and reacting for 2~4 hours after the dropwise adding of the aqueous alkali solution is finished;
(3) After the reaction is finished, adding water into the reaction kettle according to the condition that the adding amount of stearic acid accounts for 10 to 20 percent of the total amount of the raw materials;
(4) And (4) shearing and emulsifying the product obtained in the step (3) at a high speed to obtain a final product.
3. The preparation method of the solid-liquid mixed foam stabilizer according to claim 2, wherein the stearic acid is added in an amount of 10 to 20% based on 100% by mass of the total of the organic solvent, stearic acid, calcium carbonate particles, an aqueous alkali solution and water, the mass ratio of the organic solvent to the stearic acid is 1.
4. The preparation method of the solid-liquid mixed foam stabilizer according to claim 2, wherein in the step (1), the organic solvent is at least one of propylene glycol and ethylene glycol.
5. The preparation method of the solid-liquid mixed foam stabilizer according to claim 2, wherein in the step (2), the aqueous alkali solution is at least one of potassium hydroxide and sodium hydroxide.
6. The preparation method of the solid-liquid mixed foam stabilizer according to claim 2, wherein in the step (4), the shear emulsification rate is 10000 to 20000r/min, and the emulsification time is 30 to 60min.
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| US5356544A (en) * | 1992-09-06 | 1994-10-18 | Electrochemical Industries (Frutarom) Ltd. | Method for the preparation of metal soap aqueous dispersions |
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| US5356544A (en) * | 1992-09-06 | 1994-10-18 | Electrochemical Industries (Frutarom) Ltd. | Method for the preparation of metal soap aqueous dispersions |
| US5696174A (en) * | 1995-02-14 | 1997-12-09 | Allied Foam Tech Corporation | Stable and water-resistant aqueous foam composition |
| CN102746841A (en) * | 2012-06-29 | 2012-10-24 | 中国石油大学(华东) | Nanoparticle-added composite foam system used for oil and gas field and preparation method thereof |
| CN102863252A (en) * | 2012-10-22 | 2013-01-09 | 南通新邦化工科技有限公司 | Foaming-stabilizing dispersion agent for foamed cement insulation board |
| CN111253779A (en) * | 2020-01-19 | 2020-06-09 | 扬州大学 | Particle foam stabilizer and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| "Preparation and characterization of coverage-controlled CaCO3 nanoparticles";Li Yang等;《Journal of Colloid and Interface Science》;20100515;第345卷(第2期);第169页2.2 Surface coating * |
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