CN115387115A - Environment-friendly high-alkali-resistance mercerizing penetrating agent, preparation method and application thereof - Google Patents
Environment-friendly high-alkali-resistance mercerizing penetrating agent, preparation method and application thereof Download PDFInfo
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- CN115387115A CN115387115A CN202111638600.7A CN202111638600A CN115387115A CN 115387115 A CN115387115 A CN 115387115A CN 202111638600 A CN202111638600 A CN 202111638600A CN 115387115 A CN115387115 A CN 115387115A
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- parts
- alkali
- mercerizing
- resistant
- isooctanol
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/262—Sulfated compounds thiosulfates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention relates to the technical field of D06M13/322, in particular to an environment-friendly high-alkali-resistance mercerizing penetrating agent, a preparation method and application thereof. The environment-friendly high-alkali-resistance mercerizing penetrating agent comprises, by weight, 55-65 parts of isooctanol, 40-50 parts of sulfating reagent, 7-10 parts of urea, 1-5 parts of potassium permanganate, 75-85 parts of water and 40-50 parts of sodium hydroxide aqueous solution. The penetrant prepared by the method solves the problem of isooctanol residue, reduces the wastewater treatment burden of octanol contained in discharged working solution after being used by downstream customers, solves the problem of separation of residual isooctanol in an aqueous system, improves the cotton cloth permeability and alkali resistance (up to 380 g/L) under the condition of low concentration, and does not generate ammonia odor. In the reaction process, residual sulfamic acid and potassium permanganate form a strong oxidant, no acid is required to be added additionally, and the produced sodium isooctanoate is colorless and yellow liquid and cannot influence the appearance of the product.
Description
Technical Field
The invention relates to the technical field of D06M13/322, in particular to an environment-friendly high-alkali-resistance mercerizing penetrating agent, a preparation method and application thereof.
Background
In the textile industry, the mercerizing penetrant is used for cotton cloth mercerizing, and can accelerate the penetration of high-concentration alkali liquor into cotton fibers, so that the tension of the fabric is enhanced (the fabric is prevented from shrinking), and the darkening and brightening effects of stable after-treatment are facilitated. For example, CN200810024364 reacts isooctanol and sulfamic acid at 100-130 ℃ for 5-7h to obtain the penetrant, however, the penetrant isooctanol obtained by the method has low conversion rate, the problem of octanol residue exists, the application effect is influenced, and meanwhile, the method has long preparation time and low production efficiency.
Disclosure of Invention
Aiming at some problems in the prior art, the first aspect of the invention provides an environment-friendly high alkali-resistant mercerizing penetrating agent, which comprises the following raw materials, by weight, 55-65 parts of isooctanol, 40-50 parts of a sulfating agent, 7-10 parts of urea, 1-5 parts of potassium permanganate, 75-85 parts of water and 40-50 parts of a sodium hydroxide aqueous solution.
In one embodiment, the molar ratio of isooctanol to sulfating agent is 1: (1-1.1), preferably 1.
In one embodiment, the environmentally-friendly alkali-resistant mercerizing penetrant is prepared from 60 parts by weight of isooctanol, 45 parts by weight of sulfating agent, 9 parts by weight of urea, 2 parts by weight of potassium permanganate, 80 parts by weight of water and 46 parts by weight of sodium hydroxide aqueous solution.
In one embodiment, the raw materials for preparing the environment-friendly high alkali-resistant mercerizing penetrant further comprise 22-28 parts by weight of an auxiliary agent.
Preferably, the auxiliary agent is a defoaming agent and/or a solvent.
Preferably, the defoaming agent is a silicone defoaming agent.
Preferably, the solvent is an organic alcohol solvent and/or an organic acid ester solvent, preferably an organic acid ester solvent.
Preferably, the organic alcohol solvent is selected from one or more of propylene glycol, glycerol, dipropylene glycol and ethanol.
Preferably, the organic acid ester solvent is ethylene glycol diacetate.
Preferably, the weight ratio of the solvent to the defoaming agent is 10 (0.5-1.5), preferably 10.
In experiments, the applicant finds that the mercerized penetrant has problems of crystal precipitation, turbid appearance, haziness and the like in a low-temperature environment, and affects the application of the penetrant, and probably the main component in the product is water-soluble sodium isooctyl sulfate, and the penetrant comprises part of isooctyl sulfate and a defoaming agent, is a water-organic matter homogeneous system, and under the condition of low temperature, the compatibility of the organic system and water is reduced, so that the product appearance is such as chromatography, haziness and haziness, and the like, which causes inconvenience for customers to use, and simultaneously, the mercerized penetrant can be precipitated in high-concentration alkali liquor under the condition of instability. The applicant has unexpectedly found in a series of subsequent studies that when some organic alcohol solvents and/or organic acid ester solvents, especially organic acid ester solvents, are added, the organic acid ester solvents, especially organic acid ester solvents are ethylene glycol diacetate, the solvent is environmentally friendly and low in price, the problem of crystal precipitation of the penetrant in a low-temperature environment is solved, the penetrant is not limited by using conditions, the penetrant still has certain alkali resistance under the low-temperature condition, the addition of ethylene glycol diacetate can avoid the growth of crystal nuclei or control the growth rate of the crystal nuclei to be extremely low, and molecules stably exist in an aqueous solution at the low temperature.
The isooctyl alcohol described herein has a purity of greater than 99.8wt%.
In one embodiment, the sulfating agent is chlorosulfonic acid and/or sulfamic acid, preferably sulfamic acid.
The concentration of the aqueous sodium hydroxide solution described herein is not particularly limited and may be routinely selected by those skilled in the art.
In one embodiment, the concentration of the aqueous sodium hydroxide solution is 45 to 55wt%, preferably 50wt%.
In the prior art, isooctyl ammonium sulfate is synthesized at 150 ℃ by isooctyl alcohol and sulfamic acid under the catalysis of urea, however, the conversion rate of the isooctyl alcohol is not high in the reaction, the problem of higher octanol residue is solved, meanwhile, the residual quantity of sulfamic acid is also higher, the cost is increased, in the using process of the penetrant obtained by the method, because the water solubility of the isooctyl alcohol is low, cotton cloth is in the continuous mercerization process, namely, in the continuous treatment of high-concentration alkali liquor, the octanol is separated out in the high-concentration alkali liquor and is adhered to the fabric, certain inconvenience is caused to the color fixation and other subsequent treatments of the fabric, if the penetrant is not discovered or treated in time, color fixation spots or uneven color of the fabric can be caused, rework is needed, the cloth scrapping risk can be faced under serious conditions, the product performance is limited, and the alkali resistance is mostly about 250 g/L. In addition, the residual of isooctanol causes higher sewage treatment cost, and the applicant finds that the problem of the residual of isooctanol is obviously reduced by adding potassium permanganate in the research of the mercerizing penetrant, and solves the problem of high residual content of isooctanol in the prior art.
The second aspect of the invention provides a preparation method of an environment-friendly high alkali-resistant mercerizing penetrating agent, which comprises the following steps: mixing and heating isooctanol, a sulfating reagent and urea, stopping reaction when the temperature of a heating device is raised to 125-135 ℃, keeping the temperature for 2.5-3.5h when the temperature of a reaction system falls back to 145-155 ℃, then adding water to enable the temperature of the reaction system to be 75-85 ℃, adding potassium permanganate, then adding a sodium hydroxide aqueous solution for neutralization, simultaneously vacuumizing to remove ammonia gas, then adding the rest water, and sieving to obtain the catalyst.
In the application, when the temperature of a heating device is raised to 125-135 ℃, because isooctyl alcohol and a sulfating reagent are subjected to exothermal reaction, the temperature of a reaction system is raised, and in the experimental process, when the temperature of the reaction system falls back to 145-155 ℃, the reaction is carried out again in a heat preservation manner.
The reaction system refers to the reaction system of isooctanol and sulfating agent under the action of urea.
As is known to those skilled in the art, the higher the content of sulfamic acid within a certain range, the higher the permeability of the mercerizing penetrant obtained, when the molar ratio of isooctanol to sulfamic acid is 1:1.2, the higher the permeability can be maintained, when the molar ratio of isooctanol to sulfamic acid is lower than 1:1.2, and the applicants have found unexpectedly that in the preparation method of the present application, the temperature is first raised to 125-135 ℃ for reaction, and then the reaction system is maintained at 145-155 ℃ for reaction, which results in the permeability of the mercerizing penetrant obtained so that the higher permeability is maintained when the molar ratio of isooctanol to sulfamic acid is 1:1, and the wetting time is lower than 3 s.
In one embodiment, after the potassium permanganate is added, stirring is carried out for 20-30min, preferably for 25min.
The applicant has surprisingly found that the residual of octanol can be further reduced by stirring for 20-30min after the addition of potassium permanganate, and the applicant believes that the possible reason is to avoid the influence of the fatty chain in the sodium isooctyl sulfate in the reaction system on the residual isooctanol under the stirring condition to reduce the conversion of the residual isooctanol into isooctanoic acid.
In one embodiment, the screened mesh size is 200-300 mesh, preferably 250 mesh.
In one embodiment, the preparation method of the environmentally-friendly high alkali-resistant mercerizing penetrant comprises the following steps: mixing and heating isooctyl alcohol, a sulfating reagent and urea, stopping reaction when the temperature of a heating device is raised to 130 ℃, keeping the temperature for 2.5-3.5h when the temperature of a reaction system falls back to 150 ℃, then adding water to ensure that the temperature of the reaction system is 80 ℃, adding potassium permanganate, stirring for 25min, then adding a sodium hydroxide aqueous solution, neutralizing, vacuumizing to remove ammonia gas, then adding the rest water, and sieving to obtain the catalyst.
In one embodiment, after sieving, the adjuvant is added and mixed well.
The third aspect of the invention provides an application of the environment-friendly high alkali-resistant mercerizing penetrating agent in mercerizing.
Compared with the prior art, the invention has the following beneficial effects:
(1) When the sulfating reagent is sulfamic acid, the yield and the purity of the obtained sodium isooctyl sulfate are high;
(2) According to the method, by reacting isooctanol and sulfamic acid at 130 ℃, and then carrying out heat preservation reaction on a system at 150 ℃, the technical resistance of poor permeability of the mercerizing penetrant caused by low content of sulfamic acid in the prior art is solved;
(3) The addition of a certain amount of potassium permanganate in the application solves the technical problem that in the prior art, after the reaction of sulfamic acid and isooctanol, isooctanol residue affects the mercerization effect of cotton cloth;
(4) In the reaction process, when the concentration of the sodium hydroxide aqueous solution is 45-55wt%, the neutralization efficiency is high, and the influence of manganese dioxide in a suspension state on the conversion of certain water-soluble sodium isooctanoate in the stirring operation process of adding potassium permanganate in the previous stage is avoided;
(5) After potassium permanganate is added, stirring is carried out for 20-30min, and the residue of octanol is further reduced;
(6) The penetrant prepared by the method solves the problem of isooctanol residue, reduces the wastewater treatment burden of octanol contained in discharged working solution after being used by downstream customers, solves the problem of separation of residual isooctanol in an aqueous system, improves the cotton cloth permeability and alkali resistance (up to 380 g/L) under the condition of low concentration, and does not generate ammonia odor. In the reaction process, the residual sulfamic acid and potassium permanganate form a strong oxidant, no acid is required to be added additionally, and the produced sodium isooctanoate is colorless and yellow liquid and cannot influence the appearance of the product.
Detailed Description
The present invention will be described below by way of specific embodiments, but is not limited to the specific examples given below.
Examples
The isooctanols in the examples all had a purity of greater than 99.8 wt.%.
Example 1
The embodiment 1 of the invention provides an environment-friendly high-alkali-resistance mercerizing penetrating agent, which is prepared from the following raw materials in parts by weight:
60 parts of isooctanol, 45 parts of sulfamic acid, 9 parts of urea, 80 parts of water, 2 parts of potassium permanganate, 46 parts of 50wt% sodium hydroxide aqueous solution, 3 parts of acetic acid, 10 parts of ethylene glycol diacetate and 1 part of defoaming agent.
The defoaming agent is an organic silicon defoaming agent which is purchased from Nanjing Desheng and has the brand number of DS-2590.
The preparation method of the environment-friendly high alkali-resistant mercerizing penetrant comprises the following steps:
mixing and heating isooctyl alcohol, sulfamic acid and urea, stopping reaction when the temperature of a heating device is raised to 130 ℃, keeping the temperature for 3 hours when the temperature of a reaction system falls back to 150 ℃, then adding water to reduce the temperature to 80 ℃, adding potassium permanganate, stirring for 25min, then dropwise adding a sodium hydroxide aqueous solution, neutralizing, simultaneously vacuumizing to remove ammonia gas, then adding water, sieving by a 250-mesh sieve, adding ethylene glycol diacetate and a defoaming agent, and uniformly mixing to obtain the catalyst.
Example 2
The embodiment 2 of the invention provides an environment-friendly high-alkali-resistance mercerizing penetrating agent which is prepared from the following raw materials in parts by weight:
67 parts of isooctanol, 45 parts of sulfamic acid, 9 parts of urea, 80 parts of water, 46 parts of 50wt% sodium hydroxide aqueous solution, 3 parts of acetic acid, 10 parts of triethylene glycol monobutyl ether and 1 part of defoaming agent.
The antifoam was the same as in example 1.
The preparation method of the environment-friendly high alkali-resistant mercerizing penetrating agent is the same as that in example 1, except that the steps of adding potassium permanganate and stirring for 25min are omitted.
Examples 3 to 12
An environment-friendly high-alkali-resistance mercerizing penetrating agent is the same as that in example 1 in specific implementation mode, except that ethylene glycol diacetate is replaced correspondingly, and specific replacement conditions are as shown in the following table.
| Example 3 | Dimethylacetamide |
| Example 4 | Ethylene glycol monobutyl ether |
| Example 5 | Ethylene glycol butyl ether |
| Example 6 | Propylene glycol methyl ether acetate |
| Example 7 | Acetone (II) |
| Example 8 | Propylene glycol |
| Example 9 | Glycerol |
| Example 10 | Dipropylene glycol |
| Example 11 | Methanol |
| Example 12 | Ethanol |
The preparation method of the environment-friendly high-alkali-resistance mercerizing penetrating agent is the same as that in example 1, except that ethylene glycol diacetate is replaced by a corresponding substance.
Performance evaluation
1. Isooctanol residual quantity: the content of isooctanol in the penetrants obtained in example 1 and example 2 was measured by gas chromatography, respectively, and the results are shown in table 1.
2. Alkali resistance: the alkaline resistance of the penetrants of example 1 and example 2 was tested, the amount of penetrant used was 5g/L, and the highest concentration of sodium hydroxide that remained without precipitation for 24 hours was recorded, and the results are shown in Table 1.
3. And (3) permeability: the standard canvas sheet 1 is opened with 4,5g/L of the penetrant dosage of the example 1 and the example 2, the average value is obtained by measuring three times by using a stopwatch after standing for 5min under the condition of 300g/L of sodium hydroxide working solution, and the result is shown in the table 1, wherein, the wetting time refers to the time that the surface of the canvas sheet is just immersed by the alkali liquor, and the settling time refers to the time (the working solution) from the contact of the canvas sheet with the alkali liquor to the settling of the canvas sheet to the bottom of the beaker.
TABLE 1
4. Low temperature resistance: the penetrants obtained from examples 1-12 are placed in an environment at 5 ℃ for 7 days, and the appearance of the product is recorded, and the results are shown in Table 2.
TABLE 2
Claims (10)
1. An environment-friendly high-alkali-resistance mercerizing penetrating agent is characterized in that the preparation raw materials comprise, by weight, 55-65 parts of isooctanol, 40-50 parts of sulfating reagent, 7-10 parts of urea, 1-5 parts of potassium permanganate, 75-85 parts of water and 40-50 parts of sodium hydroxide aqueous solution.
2. The environmentally friendly, highly alkali-resistant mercerizing penetrant according to claim 1, wherein the molar ratio of isooctanol to sulfating agent is 1: (1-1.1).
3. The environmentally friendly highly alkali-resistant mercerizing penetrant according to claim 2, wherein the concentration of the aqueous solution of sodium hydroxide is 45-55wt%.
4. The environmentally friendly high alkali resistant mercerizing penetrant according to any one of claims 1-3, wherein the raw materials for preparing the environmentally friendly high alkali resistant mercerizing penetrant further comprise 22-28 parts by weight of an auxiliary agent.
5. The environmentally friendly, high alkali resistant mercerizing penetrant according to claim 4, wherein the auxiliary agent is defoaming agent and/or solvent.
6. The environmentally friendly high alkali resistant mercerizing penetrant according to claim 5, wherein the solvent is organic alcohol solvent and/or organic acid ester solvent.
7. A method for preparing the environmentally friendly high alkali resistant mercerizing penetrant according to any one of claims 1-3, which comprises: mixing and heating isooctanol, a sulfating reagent and urea, stopping reaction when the temperature of a heating device is raised to 125-135 ℃, keeping the temperature for 2.5-3.5h when the temperature of a reaction system falls back to 145-155 ℃, then adding water to enable the temperature of the reaction system to be 75-85 ℃, adding potassium permanganate, then adding a sodium hydroxide aqueous solution for neutralization, simultaneously vacuumizing to remove ammonia gas, then adding the rest water, and sieving to obtain the catalyst.
8. The method for preparing environment-friendly alkali-resistant mercerizing penetrant according to claim 7, wherein potassium permanganate is added and then stirred for 20-30min.
9. The method for preparing environment-friendly high alkali-resistant mercerizing penetrant according to claim 8, wherein the size of the screened mesh is 200-300 meshes.
10. Use of the environmentally friendly highly alkali-resistant mercerizing penetrant according to any one of claims 1-6 in mercerization.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111638600.7A CN115387115B (en) | 2021-12-29 | 2021-12-29 | Environment-friendly high-alkali-resistance mercerizing penetrating agent, preparation method and application thereof |
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| CN202111638600.7A CN115387115B (en) | 2021-12-29 | 2021-12-29 | Environment-friendly high-alkali-resistance mercerizing penetrating agent, preparation method and application thereof |
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| CN115387115B CN115387115B (en) | 2023-06-06 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6269880A (en) * | 1985-09-16 | 1987-03-31 | 一方社油脂工業株式会社 | Marcerizing and penetrating agent |
| CN101235001A (en) * | 2007-12-21 | 2008-08-06 | 王伟松 | Method for synthesizing aliphatic alcohol sulfate |
| CN101285263A (en) * | 2008-06-06 | 2008-10-15 | 江苏省海安石油化工厂 | Production process for environment protection type alkali resistance penetrating agent |
| CN102653921A (en) * | 2012-04-26 | 2012-09-05 | 天津达一琦精细化工有限公司 | Alkali-resisting penetrating agent for cotton fabric mercerization |
| CN109537273A (en) * | 2018-12-15 | 2019-03-29 | 广东传化富联精细化工有限公司 | Alkaline-resisting low bubble environment-friendly type silkete penetrating agent of one kind and preparation method thereof |
-
2021
- 2021-12-29 CN CN202111638600.7A patent/CN115387115B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6269880A (en) * | 1985-09-16 | 1987-03-31 | 一方社油脂工業株式会社 | Marcerizing and penetrating agent |
| CN101235001A (en) * | 2007-12-21 | 2008-08-06 | 王伟松 | Method for synthesizing aliphatic alcohol sulfate |
| CN101285263A (en) * | 2008-06-06 | 2008-10-15 | 江苏省海安石油化工厂 | Production process for environment protection type alkali resistance penetrating agent |
| CN102653921A (en) * | 2012-04-26 | 2012-09-05 | 天津达一琦精细化工有限公司 | Alkali-resisting penetrating agent for cotton fabric mercerization |
| CN109537273A (en) * | 2018-12-15 | 2019-03-29 | 广东传化富联精细化工有限公司 | Alkaline-resisting low bubble environment-friendly type silkete penetrating agent of one kind and preparation method thereof |
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| CN115387115B (en) | 2023-06-06 |
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