CN110776601B - Preparation method and application of anti-staining agent - Google Patents
Preparation method and application of anti-staining agent 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
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Abstract
The invention discloses a preparation method of an anti-staining agent, which comprises the following steps: under the action of an initiator, maleic anhydride, acrylic acid and allyl alcohol polyoxyalkyl ether as an active monomer are subjected to polymerization reaction, and the obtained water-soluble copolymer MA-AA-F6 is used as an anti-staining agent. The invention also discloses the application of the staining resistant agent, which is used for preparing a soaping agent, and the preparation method of the soaping agent comprises the following steps: and uniformly mixing the nonionic surfactant, the water-soluble copolymer MA-AA-F6 and water to obtain the soaping agent. The invention can solve the problem of serious staining of the common stain-resistant agent in the market due to poor dispersion and chelating performance on one hand, and can solve the problem of limited marketization application due to high cost on the other hand.
Description
Technical Field
The invention belongs to the technical field of textile printing and dyeing auxiliaries, and particularly relates to preparation and application of an anti-staining agent.
Background
It is known that reactive dye-printed fabrics are generally subjected to a soaping treatment, the main purpose of which is to remove the hydrolysed dyes, unfixed dyes and other impurities from the fibres and to prevent them from sticking back to the surface of the fabric, on the one hand to improve the wet crockfastness and washfastness of the dyed fabric and on the other hand to prevent the fabric from becoming stained again. Most common anti-staining agents in the current market have the problems of incomplete removal of floating color, serious staining and the like, namely, the problems of poor anti-staining effect and the like caused by poor dispersion and chelation performance; while the MA-AA-NVP anti-staining agent (maleic anhydride-acrylic acid-N-vinyl pyrrolidone terpolymer) can effectively solve the problems, the raw material cost is too high, and the marketable application is severely limited, so that an anti-staining agent with excellent anti-staining performance and low cost is urgently needed in the market.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method and application of an anti-staining agent, and by adopting the method, the cost can be reduced, and the problem of serious staining caused by poor dispersion and chelation performance can be avoided.
In order to solve the technical problems, the invention provides a preparation method of a staining resistant agent, which comprises the following steps:
under the action of an initiator (in an aqueous solution of the initiator), maleic anhydride, acrylic acid and allyl alcohol polyoxyalkyl ether (F6) serving as an active monomer are subjected to polymerization reaction at the temperature of 80 +/-5 ℃ for 2 +/-0.5 hours to obtain a water-soluble copolymer MA-AA-F6 (which is a water-soluble copolymer with good dispersion and chelating properties), and the water-soluble copolymer MA-AA-F6 is an anti-staining agent;
maleic anhydride: acrylic acid: allyl alcohol polyoxyalkyl ether = 2;
maleic anhydride, acrylic acid: the sum of the masses of the allyl alcohol polyoxyalkyl ethers is called the total mass of the monomers;
the initiator accounts for 3-6% (mass%) of the total mass of the monomers.
As an improvement of the method for preparing the anti-staining agent, the method comprises the following steps
(1) Firstly, adding water into maleic anhydride, stirring until the maleic anhydride is dissolved, then heating to (65 +/-5) DEG C under the protection of inert gas, adjusting the pH value to 6.0-6.5, and adding allyl alcohol polyoxyalkyl ether (F6);
under the protection of inert gas, heating to 80 +/-5 ℃, simultaneously dropwise adding acrylic acid and an initiator aqueous solution (namely, 2 simultaneously and respectively starting and finishing dropwise adding), wherein the dropwise adding time is (2 +/-0.2) h, and after dropwise adding, carrying out heat preservation reaction for (2 +/-0.5) h;
the mass concentration of the initiator in the initiator aqueous solution is 6-8%;
remarks explanation: when water is added to maleic anhydride, the amount of water is only required to ensure that the maleic anhydride can be dissolved, and the following maleic anhydride is preferred: water =1 (mass ratio).
The whole step (1) is carried out under the protection of inert gas.
(2) And cooling the obtained reaction product to room temperature to obtain the water-soluble copolymer MA-AA-F6.
As a further improvement of the method for preparing the anti-staining agent of the present invention: the initiator is at least one of sodium persulfate, potassium persulfate and ammonium persulfate.
The invention also provides the application of the stain resistant agent: the method for preparing the soaping agent comprises the following steps:
uniformly mixing a nonionic surfactant, a water-soluble copolymer MA-AA-F6 and water to obtain a soaping agent;
the mass sum of the nonionic surfactant and the water-soluble copolymer MA-AA-F6 accounts for 18-22% of the total mass of the soaping agent (namely, the solid content is 18-22%).
Improvement as the use of the stain repellent of the present invention: the nonionic surfactant consists of fatty alcohol-polyoxyethylene ether AEO-7 and fatty alcohol-polyoxyethylene ether AEO-25;
fatty alcohol polyoxyethylene ether AEO-7: fatty alcohol-polyoxyethylene ether AEO-25: water-soluble copolymer MA-AA-F6=1, mass ratio of 12.
In the invention, the allyl alcohol polyoxy alkyl ether as an active monomer has good solubilization, contains a large amount of O in a molecular structure, and can form a hydrogen bond with a hydrolyzed dye; the carboxylate radical in the MA-AA-F6 terpolymer can provide electrostatic action and adsorption sites, and can powerfully adsorb and disperse solid particles to prevent redeposition. Namely, the water-soluble copolymer MA-AA-F6 serving as the anti-staining agent prepared by the invention has the advantages of excellent anti-staining performance (namely, good dispersion and chelating performance), low price, easiness in popularization and application and the like.
The price of allyl alcohol polyoxyalkyl ether (F6) is only 30% of that of N-vinylpyrrolidone.
The water-soluble copolymer MA-AA-F6 can be compounded with a nonionic surfactant to prepare a soaping agent, is used for soaping reactive dyes, and has excellent floating and stain-proof removal capabilities. Namely, the soaping agent finally obtained by the invention has excellent cleaning function to the reactive dye, and has the characteristics of excellent performance and low price.
Therefore, the invention can solve the problem of serious staining of the common stain-resistant agent in the market due to poor dispersion and chelation performance on one hand, and can solve the problem of limited marketization application due to high cost on the other hand.
In conclusion, the method has the advantages of simple process, low cost, convenient implementation and operation, contribution to industrial large-scale production, great economic significance and good practical performance, and wide application prospect in the soaping agent for the reactive dye.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
in the following cases:
maleic anhydride, acrylic acid and allyl alcohol polyoxyalkyl ether (F6) are used as raw materials; different initiators are selected; the sum of the masses of maleic anhydride, acrylic acid, and allyl alcohol polyoxyalkyl ether (F6) is referred to as the total mass of the monomers.
O-7, i.e., fatty alcohol polyoxyethylene ether AEO-7; the EO number is 7, and the number of EO molecules,
o-25, i.e., fatty alcohol polyoxyethylene ether AEO-25, EO number is 25;
inert gas, preferably N 2 。
Example 1, a method for preparing a soaping agent, comprising the following two major steps:
1. preparing an anti-staining agent:
m (maleic anhydride): m (acrylic acid): m (allyl alcohol polyoxyalkyl ether) = 2; ammonium persulfate is used as an initiator, and accounts for 3 percent of the total mass of the monomers.
1) Adding 10g of maleic anhydride into 30g of water, dissolving at 30 ℃, then placing the mixture into a four-neck flask provided with a reflux device, raising the temperature to 65 ℃ under the protection of inert gas, adjusting the pH value to about 6.5 by using 30 percent of NaOH aqueous solution, continuously stirring for 20min, and adding 1g of allyl alcohol polyoxyalkyl ether (F6);
and under the protection of inert gas, heating to the polymerization temperature of 80 ℃, respectively and simultaneously dropwise adding 30g of acrylic acid and 18g of ammonium persulfate aqueous solution (containing 1.23g of ammonium persulfate), controlling the dropwise adding within 1.8-2 h, and keeping the polymerization temperature for reaction for 2h.
2) And after the reaction is finished, cooling to room temperature to obtain clear and transparent light yellow viscous liquid, namely the maleic anhydride-acrylic acid-allyl alcohol polyoxy alkyl ether (MA-AA-F6) water-soluble copolymer (serving as the anti-staining agent).
2. Preparing a soaping agent:
1.5g of O-7, 0.75g of O-25 and an appropriate amount of water (about 45 ml) were added to a reaction vessel, stirred at 30 ℃ to dissolve the mixture, after 10 minutes, 18g of a maleic anhydride-acrylic acid-allyl alcohol polyoxyalkyl ether (MA-AA-F6) water-soluble copolymer (terpolymer, as a stain repellent) was added, and then water was quantitatively added to 100g, and stirring was continued at that temperature for 30 minutes to prepare a soaping agent having a solid content of about 20.25%.
Example 2, a method for preparing a soaping agent, comprising the following two major steps:
1. preparing a staining inhibitor:
m (maleic anhydride): m (acrylic acid): m (allyl alcohol polyoxyalkyl ether) = 2; ammonium persulfate is used as an initiator, and accounts for 4% of the total mass of the monomers.
1) Adding 10g of maleic anhydride into 30g of water, dissolving at 30 ℃, then placing the mixture into a four-neck flask provided with a reflux device, heating the mixture to 65 ℃ under the protection of inert gas, adjusting the pH value to about 6.5 by using 30% NaOH aqueous solution, continuously stirring the mixture for 20min, and adding 2g of allyl alcohol polyoxyalkyl ether;
and continuously raising the temperature to 80 ℃ under the protection of inert gas, respectively and simultaneously dropwise adding 30g of acrylic acid and 24g of ammonium persulfate aqueous solution (containing 1.68g of ammonium persulfate), controlling the dropwise adding within 1.8-2 h, and keeping the polymerization temperature for reacting for 2h.
2) And after the reaction is finished, cooling to room temperature to obtain clear and transparent light yellow viscous liquid, namely the maleic anhydride-acrylic acid-allyl alcohol polyoxy alkyl ether (MA-AA-F6) water-soluble copolymer.
2. Preparing a soaping agent:
1.5g of O-7, 0.75g of O-25 and a proper amount of water (about 45 ml) were added to a reaction vessel, stirred at 30 ℃ to dissolve the components, after 10min, 18g of a terpolymer (anti-staining agent) of maleic anhydride-acrylic acid-allyl alcohol polyoxyalkyl ether (MA-AA-F6) was added, then water was added in an amount of 100g, and stirring was continued at the temperature for 30min to prepare a soaping agent having a solid content of about 20.25%.
Example 3, a method for preparing a soaping agent, comprising the following two major steps:
1. preparing an anti-staining agent:
m (maleic anhydride): m (acrylic acid): m (allyl alcohol polyoxyalkyl ether) = 2; ammonium persulfate is used as an initiator, and accounts for 6 percent of the total mass of the monomers.
1) Adding 10g of maleic anhydride to 30g of water, dissolving at 30 ℃, then placing the mixture into a four-neck flask provided with a reflux device, heating the mixture to 65 ℃ under the protection of inert gas, adjusting the pH value to about 6.5 by using 30% of NaOH aqueous solution, continuously stirring the mixture for 20min, and adding 3g of allyl alcohol polyoxyalkyl ether;
and under the protection of inert gas, heating to the polymerization temperature of 80 ℃, respectively and simultaneously dropwise adding 30g of acrylic acid and 36g of ammonium persulfate aqueous solution (containing 2.58g of ammonium persulfate), controlling the dropwise adding within 1.8-2 h, and keeping the polymerization temperature for reaction for 2h.
2) And after the reaction is finished, cooling to room temperature to obtain clear and transparent light yellow viscous liquid, namely the maleic anhydride-acrylic acid-allyl alcohol polyoxy alkyl ether (MA-AA-F6) water-soluble copolymer.
2. Preparing a soaping agent:
1.5g of O-7, 0.75g of O-25 and a proper amount of water (about 45 ml) are added into a reaction vessel, stirred at 30 ℃ to be dissolved, 18g of a terpolymer (anti-staining agent) of maleic anhydride-acrylic acid-allyl alcohol polyoxy alkyl ether (MA-AA-F6) is added after 10min, then water is added to a fixed amount of 100g, and stirring is continued at the temperature for 30min to prepare a soaping agent with the solid content of about 20.25%.
Example 4, a method of preparing a soaping agent, comprising the following two major steps:
1. preparing a staining inhibitor:
m (maleic anhydride): m (acrylic acid): m (allyl alcohol polyoxyalkyl ether) = 2; ammonium persulfate is used as an initiator, and accounts for 5 percent of the total mass of the monomers.
1) Adding 10g of maleic anhydride to 30g of water, dissolving at 30 ℃, then placing the mixture into a four-neck flask provided with a reflux device, heating the mixture to 65 ℃ under the protection of inert gas, adjusting the pH value to about 6.5 by using 30% NaOH aqueous solution, continuously stirring the mixture for 20min, and adding 4g of allyl alcohol polyoxyalkyl ether;
and continuously raising the temperature to 80 ℃ under the protection of inert gas, respectively and simultaneously dropwise adding 30g of acrylic acid and 31g of ammonium persulfate aqueous solution (containing 2.2g of ammonium persulfate), controlling the dropwise adding within 1.8-2 h, and keeping the polymerization temperature for reacting for 2h.
2) And after the reaction is finished, cooling to room temperature to obtain clear and transparent light yellow viscous liquid, namely the maleic anhydride-acrylic acid-allyl alcohol polyoxy alkyl ether (MA-AA-F6) water-soluble copolymer.
2. Preparing a soaping agent:
1.5g of O-7, 0.75g of O-25 and a proper amount of water (about 45 ml) are added into a reaction vessel, stirred at 30 ℃ to be dissolved, 18g of a terpolymer (anti-staining agent) of maleic anhydride-acrylic acid-allyl alcohol polyoxy alkyl ether (MA-AA-F6) is added after 10min, then water is added to a fixed amount of 100g, and stirring is continued at the temperature for 30min to prepare a soaping agent with the solid content of about 20.25%.
Comparative example 1, a method for preparing a soaping agent, comprising the following two major steps:
1. preparation of stain-proofing agent using maleic anhydride-acrylic acid copolymer:
m (maleic anhydride): m (acrylic acid) = 6; ammonium persulfate is used as an initiator, and the amount of the initiator is 4 percent of the sum of the mass of maleic anhydride and acrylic acid;
(1) 10g of maleic anhydride and 30g of water are placed in a four-neck flask provided with a reflux device, stirred to be dissolved, heated to 65 ℃ under the protection of inert gas, and the pH value is adjusted to about 6.5 by using 30% NaOH aqueous solution.
Under the protection of inert gas, when the temperature is raised to 85 ℃ of polymerization temperature, respectively and simultaneously dropping 30g of acrylic acid and 23g of ammonium persulfate aqueous solution (containing 1.6g of ammonium persulfate), controlling the dropping to be finished within 4h (2 dropping simultaneously, the dropping time is respectively about 4 h), and keeping the polymerization temperature for reaction for 6h.
(2) After the reaction is finished, cooling to room temperature to obtain clear, light, transparent and yellow viscous liquid, namely maleic anhydride-acrylic acid copolymer MA-AA (which is a conventional anti-staining agent).
2. Preparing a soaping agent:
1.5g of O-7, 0.75g of O-25 and a proper amount of water (about 45 ml) were added to a reaction vessel, stirred at 30 ℃ to dissolve the mixture, 18g of maleic anhydride-acrylic acid copolymer (MA-AA) was added after 10 minutes, the amount of water was further added to 100g, and stirring was continued at the temperature for 30 minutes to prepare a soaping agent having a solid content of about 20.25%.
Comparative example 2, a method of preparing a soaping agent:
1. preparing an anti-staining soaping agent by using a maleic anhydride-acrylic acid-N-vinyl pyrrolidone copolymer:
m (maleic anhydride): m (acrylic acid): m (N-vinylpyrrolidone) = 2.8; ammonium persulfate is used as an initiator, and the amount of the initiator is 4 percent of the sum of the mass of (maleic anhydride and + acrylic acid + N-vinyl pyrrolidone).
(1) 10g of maleic anhydride and 30g of water are placed in a four-neck flask provided with a reflux device, stirred to be dissolved, and introduced with N 2 Raising the temperature to 65 ℃ under protection, and adjusting the pH value to about 6.5 by using a 30% NaOH aqueous solution.
In N 2 Under protection, when the temperature is continuously raised to the polymerization temperature of 85 ℃,30g of acrylic acid, 25g of ammonium persulfate aqueous solution (containing 1.76g of ammonium persulfate) and 4g of N-vinyl pyrrolidone are respectively and simultaneously dripped, the dripping is finished within 1.5h, and the polymerization temperature is kept for reaction for 6h.
(2) And after the reaction is finished, cooling to room temperature to obtain clear and transparent yellow-brown viscous liquid, namely the maleic anhydride-acrylic acid-N-vinyl pyrrolidone (MA-AA-NVP) ternary water-soluble copolymer (MA-AA-NVP type anti-staining agent).
2. Preparing a soaping agent:
1.5g of O-7, 0.75g of O-25 and a proper amount of water (about 45 ml) are added into a reaction vessel, stirred at 30 ℃ to be dissolved, 18g of maleic anhydride-acrylic acid-N-vinyl pyrrolidone (MA-AA-NVP) ternary water-soluble copolymer (MA-AA-NVP type anti-staining agent) is added after 10min, then water is added to 100g, stirring is continued at the temperature for 30min, and the soaping agent with the solid content of about 20.25% is prepared.
Comparative example 3-1, 1.5g of O-7 and 0.75g of O-25 in step two in example 2 were changed to 1.5g of O-7 and 1.5g of O-25, and the remainder was identical to example 2.
Comparative example 3-2, in step two of example 2, "1.5g of O-7, 0.75g of O-25" was changed to "1.5g of O-7, 2.25g of O-25", and the remainder was the same as in example 2.
Comparative example 3-3, the "1.5g of O-7, 0.75g of O-25" in step two of example 2 was changed to "3g of O-7, 0.75g of O-25", and the remainder was the same as in example 2.
Experiment I,
1. The dispersibility and the chelatability are measured under the condition of the same solid content, and the method for testing the dispersing force and the chelating force comprises the following steps:
(1) Dispersibility test
Accurately weighing 4g of copolymer (antisticking agent) (accurate to 0.01 g) to prepare 100ml of solution, transferring 25ml of sample into a conical flask, and adding 10ml of 10% Na 2 CO 3 The solution and 30ml of deionized water, adjusted to pH about 11 with 30% NaOH, standardized with 0.1mol/L calcium acetateAnd (4) performing liquid titration, wherein the titration is performed until white precipitates are generated at the beginning and the end point is obtained after 30s without fading.
Calculating the dispersion force:
dispersion value (mg/G) = V C100.1/G (1)
In the formula: v-volume of sample consumed calcium acetate standard solution, ml;
concentration of C-calcium acetate, mol/L;
g-weight of sample, G;
100.1 molecular weight of calcium carbonate
(2) Chelatability test
Accurately weighing 2g of copolymer (anti-staining agent) (accurate to 0.01 g) to prepare 100ml of solution, transferring 25ml of sample solution into a conical flask, adding 5ml of 2% Na 2 C 2 O 4 Solution of NH 4 Cl-NH 3 (pH = 10) the buffer was adjusted to pH 10-10.5, titrated with 0.1mol/L calcium acetate standard, and the end point was reached when titration started to produce a white precipitate and no discoloration after 30 s.
Calculating the chelating force:
chelation value (mg/G) = V C100.1/G (2)
In the formula: v-volume of sample consumed calcium acetate standard solution, ml;
concentration of C-calcium acetate, mol/L;
g-weight of sample, G;
100.1 molecular weight of calcium carbonate
The dispersibility and the chelating property of the stain repellents in the examples 1, 2, 3, 4, 1 and 2 are measured by the above test method after the treatments under the same conditions; the test results are shown in table 1 below.
TABLE 1 comparison of the various properties of the copolymers (antisticking agents)
| Sample (I) | Dispersion number (mg/g) | Chelate number (mg/g) |
| Example 1 | 283.181 | 325.799 |
| Example 2 | 312.954 | 372.233 |
| Example 3 | 263.914 | 320.022 |
| Example 4 | 286.045 | 322.584 |
| Comparative example 1 | 188.417 | 194.526 |
| Comparative example 2 | 311.845 | 303.761 |
As can be seen from Table 1, the MA-AA-F6 terpolymer (anti-staining agent) has good dispersion chelation performance and the performance of the MA-AA-NVP terpolymer is equivalent to that of the NVP terpolymer by adopting the same test method under the condition of containing the same mass of active ingredients, but the cost price of F6 is far lower than that of NVP, and the MA-AA-F6 has good practicability and great economic significance.
Experiment two,
The soaping agents obtained in the examples 1 to 4 were applied to the soaping of reactive dye dyed fabrics (reactive brilliant blue KN-R type dye dyed cotton fabrics) with the soaping agent dosage of 3g/L, the bath ratio of 1 to 50, the soaping temperature of 95 ℃ and the time of 30min, and the results are shown in Table 2.
TABLE 2 comparison of soaping agent Performance
The K/S value is used for representing the staining resistance of the soaping agent, the lower the K/S value of the white cloth for the lining is, the better the staining resistance is, and otherwise, the worse the staining resistance is; the absorbance A value of the residual liquid is used for representing the content of the dye in the soap boiling residual liquid, the larger the absorbance A value of the residual liquid is, the better the cleaning capacity of the soaping agent is, and the worse the washing capacity is otherwise.
Comparative experiment, the maleic anhydride-acrylic acid soaping agent obtained in comparative example 1, the maleic anhydride-acrylic acid-N-vinylpyrrolidone soaping agent obtained in comparative example 2, and the soaping agents obtained in comparative example 3 were examined by the method described in experiment two, and the obtained K/S values were as shown in table 3.
TABLE 3
| Soaping agent | Anti-staining white cloth K/S |
| Comparative example 1 | 1.1608 |
| Comparative example 2 | 0.9106 |
| Comparative example 3-1 | 0.9703 |
| Comparative examples 3 to 2 | 0.9418 |
| Comparative examples 3 to 3 | 0.9856 |
As can be seen from tables 2 and 3, the stain resistant agent prepared by the method has excellent stain resistant capability and cleaning capability, and the fabric after soaping has good dry and wet rubbing fastness.
Finally, it is also noted that the above-mentioned list is only a few specific embodiments of the present invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (2)
1. The preparation method of the anti-staining agent is characterized by comprising the following steps:
maleic anhydride: acrylic acid: allyl alcohol polyoxyalkyl ether F6=2, mass ratio of 0.4; ammonium persulfate is used as an initiator, and accounts for 4% of the total mass of the monomers;
the method comprises the following steps:
1) Adding 10g of maleic anhydride into 30g of water, dissolving at 30 ℃, then placing the mixture into a four-neck flask provided with a reflux device, heating the mixture to 65 ℃ under the protection of inert gas, adjusting the pH value to about 6.5 by using 30% NaOH aqueous solution, continuously stirring the mixture for 20min, and adding 2g of allyl alcohol polyoxyalkyl ether F6;
continuously heating to the polymerization temperature of 80 ℃ under the protection of inert gas, respectively and simultaneously dropwise adding 24g of acrylic acid and ammonium persulfate aqueous solution containing 1.68g of ammonium persulfate, controlling the adding within 1.8 to 2h, and keeping the polymerization temperature for reaction for 2h;
2) And after the reaction is finished, cooling to room temperature to obtain clear and transparent light yellow viscous liquid, and obtaining the maleic anhydride-acrylic acid-allyl alcohol polyoxy alkyl ether MA-AA-F6 water-soluble copolymer serving as the stain inhibitor.
2. Use of the stain repellent prepared by the method of claim 1, wherein: the method for preparing the soaping agent comprises the following steps:
adding 1.5g of fatty alcohol-polyoxyethylene ether AEO-7, 0.75g of fatty alcohol-polyoxyethylene ether AEO-25 and a proper amount of water into a reaction container, stirring at 30 ℃ to dissolve, adding 18g of maleic anhydride-acrylic acid-allyl alcohol polyoxyalkyl ether MA-AA-F6 water-soluble copolymer after 10min, adding a fixed amount of water to 100g, and continuously stirring at the temperature for 30min to prepare the soaping agent with the solid content of 20.25%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0364399A2 (en) * | 1988-10-03 | 1990-04-18 | Ciba-Geigy Ag | Water soluble or water dispersible copolymers, their preparation and use |
| CN108264617A (en) * | 2017-12-30 | 2018-07-10 | 绍兴市津工科技有限公司 | A kind of chelated dispersants and preparation method thereof |
-
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0364399A2 (en) * | 1988-10-03 | 1990-04-18 | Ciba-Geigy Ag | Water soluble or water dispersible copolymers, their preparation and use |
| CN108264617A (en) * | 2017-12-30 | 2018-07-10 | 绍兴市津工科技有限公司 | A kind of chelated dispersants and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| MA-AA-NVP三元共聚物的合成及性能;赖亚琴等;《浙江理工大学学报》;20090331;第26卷(第2期);第184-188页 * |
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