CN113429505A - Odorless thickener for reactive dye printing and preparation method thereof - Google Patents
Odorless thickener for reactive dye printing and preparation method thereof Download PDFInfo
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- CN113429505A CN113429505A CN202110791739.9A CN202110791739A CN113429505A CN 113429505 A CN113429505 A CN 113429505A CN 202110791739 A CN202110791739 A CN 202110791739A CN 113429505 A CN113429505 A CN 113429505A
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- C08F2/00—Processes of polymerisation
- C08F2/32—Polymerisation in water-in-oil emulsions
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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
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
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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
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
- D06P1/5257—(Meth)acrylic acid
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Abstract
The invention discloses a tasteless thickener for reactive dye printing and a preparation method thereof. The preparation method comprises the following steps: preparing a water phase, preparing an oil phase, preparing an inverse pre-emulsion, performing inverse pre-emulsion polymerization, performing emulsion phase inversion and deodorizing. According to the invention, through the selection of the white oil, the kerosene and water in the active dye printing thickener are evaporated in the process of carrying out reduced pressure concentration on the active dye printing thickener, and the white oil is used for replacing the kerosene, so that on one hand, the smell of the thickener due to the kerosene is effectively removed, the odorless treatment is realized, on the other hand, the concentration and the salt resistance of the thickener are also improved, and the prepared thickener finished product has low water content, oil-free water phase layering phenomenon, no putrefaction due to bacteria breeding, stable performance and long shelf life.
Description
Technical Field
The invention relates to the field of textile auxiliary agents, in particular to an odorless thickening agent for reactive dye printing and a preparation method thereof.
Background
The polyacrylic acid thickener is a network-like high polymer which swells but does not dissolve in water, has strong water absorption performance, good biocompatibility, no toxicity and stable property, and is favored by the market. At present, polyacrylic acid thickening agents are mainly applied to the fields of pharmacy, coatings and adhesives, daily chemical products, printing and dyeing textiles and the like.
Most of the existing polyacrylic acid thickeners contain kerosene, such as the polyacrylic acid thickener modified by nonionic and acidic side groups disclosed in Chinese patent CN 111995718A and the preparation method thereof, wherein kerosene accounting for 0.6-0.8 times of the mass of pure water is used. Kerosene has relatively unpleasant smell, even odorless kerosene can give off the unpleasant smell, and the smell can be brought into a downstream application environment and remains on fabrics, so that the use experience of a user is influenced. In addition, the polyacrylic acid thickener has poor salt resistance, and a large amount of salt needs to be added in reactive dye printing, so that the conventional polyacrylic acid thickener cannot well meet the requirements of reactive printing.
Disclosure of Invention
The invention mainly solves the technical problem of providing the odorless thickener for reactive dye printing and the preparation method thereof, and can solve the defects of the conventional polyacrylic acid thickener in the aspect of reactive dye printing.
In order to solve the technical problems, the invention adopts a technical scheme that: provides an odorless thickener for printing reactive dyes, which comprises the following components in percentage by mass:
25-35% of an alkali solution, 18-25% of acrylic acid and/or methacrylic acid, 5-10% of acrylamide and/or methacrylamide, 1-3% of a cationic monomer, 10-20% of water, 1-3% of a crosslinking monomer, 1-5% of a long-chain alkyl acrylate, 15-25% of white oil, 1-5% of span, 3-6% of linseed oil, 2-5% of a diverting agent and 0.1-0.5% of an initiator.
In a preferred embodiment of the present invention, the cationic monomer comprises at least one of methacryloyloxyethyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, acryloyloxyethyl trimethyl ammonium chloride, acryloyloxyethyl dimethyl benzyl ammonium chloride.
In a preferred embodiment of the present invention, the crosslinking monomer is any one or two of N, N' -methylenebisacrylamide, glycidyl acrylate, glycidyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, or hydroxyethyl methacrylate.
In a preferred embodiment of the present invention, the long-chain alkyl acrylate is any one to three of dodecyl acrylate, tridecyl acrylate, tetradecyl acrylate, hexadecyl acrylate, octadecyl acrylate, and docosyl acrylate.
In a preferred embodiment of the present invention, the initiator is at least one of ammonium persulfate, sodium persulfate, or potassium persulfate.
In a preferred embodiment of the present invention, the alkali solution is at least one of an aqueous solution of sodium hydroxide, potassium hydroxide or lithium hydroxide with a mass concentration of 30 to 35%.
In a preferred embodiment of the present invention, the white oil is any one to three of 5# white oil, 7# white oil, 10# white oil, 15# white oil, 26# white oil or 32# white oil.
In order to solve the technical problem, the invention adopts another technical scheme that: the preparation method of the odorless thickener for printing the reactive dye comprises the following steps:
(1) preparing an aqueous phase: according to the formula amount, dripping acrylic acid or methacrylic acid into the alkali solution, adding acrylic acid amide or methacrylic acid amide, a cationic monomer and a crosslinking monomer after dripping, and stirring for dissolving to obtain a water phase;
(2) preparing an oil phase: weighing kerosene with the same amount as the white oil, and fully and uniformly mixing the kerosene with the long-chain alkyl acrylate, span and linseed oil in the formula according to the formula amount to prepare an oil phase;
(3) preparing an inverse pre-emulsion: transferring the oil phase prepared in the step (2) into an emulsifying kettle, and dropwise adding the water phase prepared in the step (1) into the oil phase under the conditions of shearing, stirring and emulsifying to prepare a water-in-oil type reverse phase pre-emulsion;
(4) inverse pre-emulsion polymerization: transferring the inverse pre-emulsion obtained in the step (3) into a polymerization reaction kettle, introducing nitrogen to remove oxygen, heating to a polymerization temperature, dropwise adding a mixed solution of an initiator and water in a formula amount, and preserving heat after dropwise adding is finished to finish a polymerization reaction;
(5) phase inversion of emulsion: cooling the emulsion polymerized in the step (4) to room temperature, adding a diverting agent in a formula amount, and stirring to complete phase inversion to obtain the reactive dye printing thickener;
(6) deodorizing treatment: and (3) transferring the reactive dye printing thickener obtained in the step (5) into a concentration kettle, carrying out reduced pressure distillation, removing the kerosene and water, adding the white oil with the formula amount in the distillation process, and obtaining the odorless thickener for printing the reactive dye after the kerosene and the water are distilled.
In a preferred embodiment of the present invention, in the step (4), the polymerization conditions are: the polymerization temperature is 65-80 ℃, the submitting time of the mixed liquid of the initiator and the water is 2-4 h, and the heat preservation time is 2 h.
In a preferred embodiment of the present invention, in the step (5), the process conditions of the reduced pressure distillation are as follows: the pressure is 2.0-2.7 kPa, and the temperature is 35-95 ℃.
The invention has the beneficial effects that: the invention relates to an odorless thickener for printing reactive dyes and a preparation method thereof.
Drawings
FIG. 1 is a process flow diagram of a preparation method of the odorless thickener for printing with the reactive dye.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Referring to fig. 1, an embodiment of the present invention includes:
a preparation method of an odorless thickener for reactive dye printing specifically comprises the following steps:
(1) dropwise adding 18-25% by mass of acrylic acid or methacrylic acid or a mixture of acrylic acid and methacrylic acid mixed in any proportion into 25-35% by mass of sodium hydroxide solution, potassium hydroxide solution or lithium hydroxide solution with the mass concentration of 30-35%, after dropwise addition, adding 5-10% by mass of acrylamide or methacrylamide or a mixture of acrylamide and methacrylamide mixed in any proportion, 1-3% by mass of cationic monomer and 1-3% by mass of crosslinking monomer, fully stirring for dissolving, and cooling to obtain a water phase;
by adopting the cationic monomer to participate in the polymerization reaction, a cationic group can be introduced into the macromolecular main chain of the thickening agent, and the salt resistance of the thickening agent can be improved by utilizing the ionic property of the cationic group. The cationic monomer comprises at least one of methacryloyloxyethyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, acryloyloxyethyl trimethyl ammonium chloride and acryloyloxyethyl dimethyl benzyl ammonium chloride; the crosslinking monomer is any one or two of N, N' -methylene bisacrylamide, glycidyl acrylate, glycidyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate or hydroxyethyl methacrylate.
(2) Weighing kerosene which is equal to the white oil (the kerosene which accounts for 15-25% of the formula is also weighed because the mass percentage of the white oil in the formula is 15-25%), and fully and uniformly mixing the weighed kerosene with 1-5% of long-chain alkyl acrylate, 1-5% of span and 3-6% of linseed oil to prepare an oil phase;
wherein, the acrylic acid long-chain alkyl ester is any one to three of lauryl acrylate, tridecyl acrylate, tetradecyl acrylate, hexadecyl acrylate, octadecyl acrylate and behenyl acrylate. The hydrophobic chain segment contained in the acrylic acid long-chain alkyl ester can enable a macromolecular chain to generate association, and the hydration of the acrylic acid long-chain alkyl ester and a polar group can enable the macromolecular chain to be in a stretching state, so that the macromolecular chain is physically crosslinked to form a space network structure with certain strength, the water retention performance is improved, and the thickening performance and the salt resistance of the thickening agent are improved.
The span is any one to three of span-20, span-40, span-60, span-80 or span-85;
(3) transferring the oil phase prepared in the step (2) into an emulsifying kettle, dropwise adding the water phase prepared in the step (1) into the oil phase under the condition of shearing, stirring and emulsifying at the stirring speed of 1000-5000 r/min, and continuously stirring for 30min after dropwise adding is finished to prepare the water-in-oil type inverse pre-emulsion;
(4) transferring the inverse pre-emulsion obtained in the step (3) into a polymerization reaction kettle, continuously introducing nitrogen for 15-20 min under a stirring state, discharging oxygen in the polymerization reaction kettle, heating to 65-80 ℃, dropwise adding a mixed solution of 0.1-0.2% by mass of an initiator and 10-20% by mass of deionized water, completely dripping within 2-4 h, and preserving heat at 65-80 ℃ for 2h to complete a polymerization reaction; wherein the initiator is at least one of ammonium persulfate, sodium persulfate or potassium persulfate;
(5) cooling the emulsion polymerized in the step (4) to room temperature, adding a diverting agent in a formula amount, and stirring to complete phase inversion to obtain the reactive dye printing thickener;
wherein the diverter is any 1-3 of tween-20, tween-40, tween-60, tween-80, tween-85, AEO-3, AEO-4, AEO-5, AEO-7 and AEO-9;
(6) and (3) transferring the reactive dye printing thickener obtained in the step (5) into a concentration kettle, evaporating under reduced pressure to remove the kerosene and water under the conditions that the pressure is 2.0-2.7 kPa and the temperature is 35-95 ℃, adding the white oil with the formula amount in the distillation process, and obtaining the odorless thickener for reactive dye printing after the kerosene and the water are distilled. Since kerosene has a certain odor, unpleasant odors can be emitted during the application process or on the printed fabric. White oil kerosene has an odor, but the viscosity of white oil is higher than that of kerosene, and if the white oil kerosene is directly used in the reaction, the white oil kerosene is not beneficial to the mass transfer and heat transfer of the reaction, so that the white oil kerosene cannot be directly used in the reaction system. The kerosene and water in the prepared thickening agent are evaporated, and the kerosene in the system is replaced by white oil, so that the odorless high-concentration thickening agent can be obtained, and the thickening performance and the salt resistance of the thickening agent can be improved.
The white oil is any 1-3 of 5# white oil, 7# white oil, 10# white oil, 15# white oil, 26# white oil or 32# white oil.
Example 1
220kg of acrylic acid is added into 335kg of sodium hydroxide aqueous solution (the mass fraction is 32%), after the addition, 70kg of acrylamide, 20kg of methacryloyloxyethyl trimethyl ammonium chloride, 20kg of N, N' -methylene bisacrylamide and 110kg of water are added, fully stirred, dissolved and cooled to obtain a water phase;
fully and uniformly stirring 40kg of octadecyl acrylate, 200kg of kerosene, 16kg of span 80 and 40kg of linseed oil to prepare an oil phase;
and transferring the oil phase into an emulsifying kettle, dropwise adding the water phase into the oil phase under the high-shear stirring of 1500r/min for 20 minutes, and continuously stirring for 30 minutes after the addition is finished to form the stable water-in-oil type reverse-phase pre-emulsion.
Transferring the pre-emulsion into a polymerization reaction kettle, stirring, continuously introducing nitrogen for 15-20 minutes, discharging oxygen in the reaction kettle, heating to 65 ℃, dropwise adding an ammonium persulfate aqueous solution (2kg of ammonium persulfate is dissolved by 20kg of water), dropwise adding for 2 hours at the temperature of 65-70 ℃, and after dropwise adding, keeping the temperature of 65-70 ℃ for 2 hours;
cooling the polymerized emulsion to room temperature, adding AEO-922 kg, continuing stirring, and completing phase inversion to obtain the reactive dye printing thickener;
transferring the thickener after phase inversion into a concentration kettle, reducing the pressure to 2.0kPa, distilling at 70 ℃ to evaporate about 200kg of kerosene and about 405kg of water, continuously supplementing 200kg of No. 5 white oil into the kettle in the distillation process, and obtaining the odorless high-concentration thickener for reactive dye printing after the distillation with the kerosene and the water is finished.
Example 2
220kg of acrylic acid is dropwise added into 335kg of sodium hydroxide aqueous solution (mass fraction is 32%), after the dropwise addition is finished, 70kg of acrylamide, 10kg of methacrylamide, 30kg of acryloyloxyethyldimethylbenzylammonium chloride, 10kg of N, N' -methylenebisacrylamide, 10kg of hydroxyethyl methacrylate and 110kg of water are added, fully stirred, dissolved and cooled to obtain a water phase;
fully and uniformly stirring 30kg of behenyl acrylate, 10kg of hexadecyl acrylate, 200kg of kerosene, 16kg of span 80 and 40kg of linseed oil to prepare an oil phase;
and transferring the oil phase into an emulsifying kettle, dropwise adding the water phase into the oil phase under the high-shear stirring of 2000r/min for 20 minutes, and continuously stirring for 30 minutes after the dropwise adding is finished to form the stable water-in-oil type reverse pre-emulsion.
Transferring the pre-emulsion into a polymerization reaction kettle, stirring, continuously introducing nitrogen for 15-20 minutes, discharging oxygen in the reaction kettle, heating to 65 ℃, dropwise adding an ammonium persulfate aqueous solution (2kg of ammonium persulfate is dissolved by 20kg of water), dropwise adding for 2 hours at the temperature of 65-70 ℃, and after dropwise adding, keeping the temperature of 65-70 ℃ for 2 hours;
cooling the polymerized emulsion to room temperature, adding tween-8022 kg, continuously stirring, and finishing phase inversion to obtain the reactive dye printing thickener;
transferring the thickener after the phase inversion into a concentration kettle, reducing the pressure to 2.2kPa, distilling at 80 ℃, distilling to obtain about 200kg of kerosene and about 405kg of water, continuously supplementing 200kg of No. 15 white oil into the kettle in the distillation process, and obtaining the odorless high-concentration thickener for reactive dye printing after the kerosene and the water are distilled.
Example 3
200kg of acrylic acid and 25kg of methacrylic acid are added dropwise into 340kg of sodium hydroxide aqueous solution (mass fraction is 32%), and after the addition of the acrylic acid and the methacrylic acid is finished, 70kg of acrylamide, 20kg of acryloyloxyethyl trimethyl ammonium chloride, 10kg of N, N' -methylene bisacrylamide and 110kg of water are added, fully stirred, dissolved and cooled to obtain a water phase;
fully and uniformly stirring 30kg of octadecyl acrylate, 10kg of dodecyl acrylate, 10kg of glycidyl acrylate, 200kg of kerosene, 16kg of span 80 and 40kg of linseed oil to prepare an oil phase;
and transferring the oil phase into an emulsifying kettle, dropwise adding the water phase into the oil phase under the high-shear stirring of 2500r/min for 20 minutes, and continuously stirring for 30 minutes after the addition is finished to form the stable water-in-oil type reverse pre-emulsion.
Transferring the pre-emulsion into a polymerization reaction kettle, stirring, continuously introducing nitrogen for 15-20 minutes, discharging oxygen in the reaction kettle, heating to 65 ℃, dropwise adding a sodium persulfate aqueous solution (2kg of sodium persulfate is dissolved by 20kg of water), dropwise adding for 2 hours at the temperature of 65-70 ℃, and after dropwise adding, keeping the temperature at 65-70 ℃ for 2 hours;
cooling the polymerized emulsion to room temperature, adding AEO-422 kg, continuously stirring, and completing phase inversion to obtain the reactive dye printing thickener;
transferring the thickener after the phase inversion into a concentration kettle, reducing the pressure to 2.5kPa, distilling at 90 ℃ to distill about 200kg of kerosene and about 410kg of water, continuously supplementing 200kg of No. 10 white oil into the kettle in the distillation process, and obtaining the odorless high-concentration thickener for reactive dye printing after the distillation of the kerosene and the water is finished.
And (3) performance testing: the thickeners prepared in examples 1 to 3 above were subjected to the following performance tests:
thickening value: 4.0g of the sample of example 1 to 3 was accurately weighed, diluted with 100mL of distilled water, and the viscosity was measured with a model NDJ-1 rotational viscometer using a number 4 spindle at a rotation speed of 6 rpm.
Salt resistance value: 4.5g of the sample of example 1 to 3 was weighed out accurately, diluted with 100mL of distilled water, and 11.5g of a 2mol/L aqueous solution of sodium chloride was added thereto, and the viscosity was measured with a rotational viscometer of type NDJ-1 using a number 4 spindle at a rotation speed of 6 rpm.
The test results are shown in the following table.
| Thickening value | Salt tolerance value | |
| Example 1 | 110000cps | 61000cps |
| Example 2 | 100000cps | 60000cps |
| Example 3 | 120000cps | 61500cps |
The invention adopts a reverse emulsion polymerization method to copolymerize a cationic monomer, long-chain alkyl acrylate, linseed oil and an acrylic hydrophilic monomer, so that the salt resistance and the thickening performance of the thickening agent are improved, and the adsorption rate and the fixation rate of the fabric to the dye can be improved.
In the polymerization reaction stage, the kerosene is used as an oil phase solvent, the thickener after polymerization is subjected to reduced pressure distillation, the kerosene and water in the product are distilled off, and the white oil with the same weight as the kerosene is continuously supplemented in the distillation process to replace the kerosene, so that the smell of the thickener due to the kerosene is effectively removed, the odorless treatment is realized, the content of macromolecular polymers in the finished thickener product is up to more than 68%, and the thickening performance and the salt resistance are further improved. Because the finished product contains almost no water, the finished thickener has no oil-water phase layering phenomenon, does not decay due to bacteria breeding, and has stable performance and long shelf life.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. An odorless thickener for printing of reactive dyes is characterized by comprising the following components in percentage by mass:
25-35% of an alkali solution, 18-25% of acrylic acid and/or methacrylic acid, 5-10% of acrylamide and/or methacrylamide, 1-3% of a cationic monomer, 10-20% of water, 1-3% of a crosslinking monomer, 1-5% of a long-chain alkyl acrylate, 15-25% of white oil, 1-5% of span, 3-6% of linseed oil, 2-5% of a diverting agent and 0.1-0.5% of an initiator.
2. The odorless thickener of claim 1, wherein the cationic monomer comprises at least one of methacryloyloxyethyl trimethyl ammonium chloride, dimethyldiallylammonium chloride, acryloyloxyethyl trimethyl ammonium chloride, acryloyloxyethyl dimethyl benzyl ammonium chloride.
3. The odorless thickener of claim 1, wherein the crosslinking monomer is one or two of N, N' -methylene bisacrylamide, glycidyl acrylate, glycidyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate and hydroxyethyl methacrylate.
4. The odorless thickener of claim 1, wherein the long-chain alkyl acrylate is any one to three of dodecyl acrylate, tridecyl acrylate, tetradecyl acrylate, hexadecyl acrylate, octadecyl acrylate and docosyl acrylate.
5. The odorless thickener of claim 1, wherein the initiator is at least one of ammonium persulfate, sodium persulfate or potassium persulfate.
6. The odorless thickener according to claim 1, wherein the alkali solution is at least one of sodium hydroxide, potassium hydroxide or lithium hydroxide aqueous solution with a mass concentration of 30-35%.
7. The odorless thickener of claim 1, wherein the white oil is any one to three of No. 5 white oil, No. 7 white oil, No. 10 white oil, No. 15 white oil, No. 26 white oil or No. 32 white oil.
8. A method for preparing a non-odorous thickener for printing reactive dyes according to any of claims 1 to 7, comprising the steps of:
(1) preparing an aqueous phase: according to the formula amount, dripping acrylic acid or methacrylic acid into the alkali solution, adding acrylic acid amide or methacrylic acid amide, a cationic monomer and a crosslinking monomer after dripping, and stirring for dissolving to obtain a water phase;
(2) preparing an oil phase: weighing kerosene with the same amount as the white oil, and fully and uniformly mixing the kerosene with the long-chain alkyl acrylate, span and linseed oil in the formula according to the formula amount to prepare an oil phase;
(3) preparing an inverse pre-emulsion: transferring the oil phase prepared in the step (2) into an emulsifying kettle, and dropwise adding the water phase prepared in the step (1) into the oil phase under the conditions of shearing, stirring and emulsifying to prepare a water-in-oil type reverse phase pre-emulsion;
(4) inverse pre-emulsion polymerization: transferring the inverse pre-emulsion obtained in the step (3) into a polymerization reaction kettle, introducing nitrogen to remove oxygen, heating to a polymerization temperature, dropwise adding a mixed solution of an initiator and water in a formula amount, and preserving heat after dropwise adding is finished to finish a polymerization reaction;
(5) phase inversion of emulsion: cooling the emulsion polymerized in the step (4) to room temperature, adding a diverting agent in a formula amount, and stirring to complete phase inversion to obtain the reactive dye printing thickener;
(6) deodorizing treatment: and (3) transferring the reactive dye printing thickener obtained in the step (5) into a concentration kettle, carrying out reduced pressure distillation, removing the kerosene and water, adding the white oil with the formula amount in the distillation process, and obtaining the odorless thickener for printing the reactive dye after the kerosene and the water are distilled.
9. The method for preparing an odorless thickener for printing with reactive dye according to claim 8, wherein in the step (4), the polymerization reaction conditions are as follows: the polymerization temperature is 65-80 ℃, the submitting time of the mixed liquid of the initiator and the water is 2-4 h, and the heat preservation time is 2 h.
10. The method for preparing an odorless thickener for printing reactive dyes according to claim 8, wherein in the step (5), the process conditions of the reduced pressure distillation are as follows: the pressure is 2.0-2.7 kPa, and the temperature is 35-95 ℃.
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| CN114134732A (en) * | 2021-11-24 | 2022-03-04 | 杭州传化精细化工有限公司 | Compound thickener and preparation method thereof |
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| CN114134732A (en) * | 2021-11-24 | 2022-03-04 | 杭州传化精细化工有限公司 | Compound thickener and preparation method thereof |
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