CN113564912A - Preparation method and application of efficient cold rolling batch refining agent - Google Patents
Preparation method and application of efficient cold rolling batch refining agent Download PDFInfo
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- CN113564912A CN113564912A CN202110855634.5A CN202110855634A CN113564912A CN 113564912 A CN113564912 A CN 113564912A CN 202110855634 A CN202110855634 A CN 202110855634A CN 113564912 A CN113564912 A CN 113564912A
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- 238000007670 refining Methods 0.000 title claims abstract description 61
- 238000005097 cold rolling Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 103
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 83
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 31
- 239000008139 complexing agent Substances 0.000 claims abstract description 30
- 230000000149 penetrating effect Effects 0.000 claims abstract description 18
- 230000003213 activating effect Effects 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 75
- 238000003756 stirring Methods 0.000 claims description 71
- 239000003054 catalyst Substances 0.000 claims description 57
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 33
- 238000001816 cooling Methods 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 31
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 28
- 108010010803 Gelatin Proteins 0.000 claims description 28
- 229920000159 gelatin Polymers 0.000 claims description 28
- 239000008273 gelatin Substances 0.000 claims description 28
- 235000019322 gelatine Nutrition 0.000 claims description 28
- 235000011852 gelatine desserts Nutrition 0.000 claims description 28
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 26
- 239000012190 activator Substances 0.000 claims description 24
- -1 fatty ester amine Chemical class 0.000 claims description 24
- 239000004094 surface-active agent Substances 0.000 claims description 24
- 238000009991 scouring Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 21
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 21
- 229920000570 polyether Polymers 0.000 claims description 21
- 238000004321 preservation Methods 0.000 claims description 21
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 19
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 19
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 19
- 239000000174 gluconic acid Substances 0.000 claims description 19
- 235000012208 gluconic acid Nutrition 0.000 claims description 19
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 19
- 239000011976 maleic acid Substances 0.000 claims description 19
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 19
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 17
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 17
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 14
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- 238000004061 bleaching Methods 0.000 claims description 13
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical group NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 12
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 12
- 125000000217 alkyl group Chemical group 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000009999 singeing Methods 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 29
- 239000003513 alkali Substances 0.000 abstract description 27
- 239000004744 fabric Substances 0.000 abstract description 19
- 230000001804 emulsifying effect Effects 0.000 abstract description 3
- 239000000835 fiber Substances 0.000 abstract description 2
- 239000012466 permeate Substances 0.000 abstract 1
- 230000003381 solubilizing effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000002738 chelating agent Substances 0.000 description 6
- 235000011121 sodium hydroxide Nutrition 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- 239000012752 auxiliary agent Substances 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 5
- 229920001897 terpolymer Polymers 0.000 description 5
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 4
- 235000017491 Bambusa tulda Nutrition 0.000 description 4
- 241001330002 Bambuseae Species 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 4
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 4
- 239000011425 bamboo Substances 0.000 description 4
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 240000005002 Erythronium dens canis Species 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 210000002268 wool Anatomy 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001408 amides Chemical group 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000002337 anti-port Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- ADOOKKARKXDTNS-UHFFFAOYSA-L cobalt tetracarboxyphthalocyanine Chemical compound [H+].[H+].[H+].[H+].[Co+2].N1=C(N=C2C3=CC=C(C=C3C(=NC=3C4=CC=C(C=C4C(=N4)N=3)C([O-])=O)[N-]2)C([O-])=O)C2=CC(=C([O-])[O-])C=CC2=C1N=C1C2=CC(C([O-])=O)=CC=C2C4=N1 ADOOKKARKXDTNS-UHFFFAOYSA-L 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
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Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/10—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
- D06L4/13—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen using inorganic agents
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/10—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
- D06L4/12—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen combined with specific additives
Abstract
The invention discloses a preparation method and application of an efficient cold rolling batch refining agent, wherein the preparation method comprises the following steps: (a) preparing a high-efficiency penetrating agent; (b) preparing a hydrogen peroxide low-temperature activating agent; (c) preparing a metal complexing agent; (d) and (4) preparing a refining agent. The refining agent prepared by the invention not only has the capability of enabling the refining solution to quickly permeate, resists high-concentration alkali liquor and has good emulsifying, dispersing and solubilizing capabilities, but also enables hydrogen peroxide to be stable in the high-concentration alkali liquor, and the scoured and bleached fabric has better capillary effect and whiteness and lower fiber damage degree.
Description
Technical Field
The invention relates to the technical field of fabric printing and dyeing pretreatment, in particular to a preparation method and application of an efficient cold-rolling batch refining agent.
Background
Compared with the conventional process, the cold pad-batch pretreatment process has the advantages that the temperature is low, the alkali concentration is high, the penetration of the alkali-oxygen solution to the cotton grey cloth is more difficult, and particularly the emulsifying capacity to grease and wax is low at low temperature; therefore, higher demands are made on scouring and bleaching aids. At present, the cold pad-batch pretreatment process has a plurality of advantages, but has the problem that the color difference is difficult to overcome due to inconsistent whiteness and capillary effect of the inside and outside of edges. Therefore, the market needs to further develop an efficient pretreatment agent, so that the cold pad-batch and short-flow scouring and bleaching process is continuously perfected to meet the needs of the efficient short-flow process and the popularization and application of the cold pad-batch pretreatment process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method and application of an efficient cold rolling batch refining agent.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an efficient cold rolling stack refining agent comprises the following steps:
(a) preparing a high-efficiency penetrating agent: under the protection of nitrogen, mixing and stirring the special EO/PO polyether, the fatty ester amine and the catalyst I in a reaction kettle to react to obtain a first intermediate, adding maleic anhydride to continue the reaction to obtain a second intermediate, and cooling and adjusting the pH value to 6-8 to obtain the high-efficiency penetrating agent;
(b) preparing a hydrogen peroxide low-temperature activating agent: adding a mixture of gelatin and ethylenediamine and copper sulfate into a reaction kettle, heating to 60 ℃, stirring and mixing, adding a catalyst II at the constant temperature for three times every 2 hours, then carrying out heat preservation reaction, and after the reaction is finished, cooling, discharging and purifying to obtain a hydrogen peroxide low-temperature activator;
(c) preparing a metal complexing agent: dissolving maleic acid and gluconic acid in hot water in a third reaction kettle, heating to 95-98 ℃, adding 1/5 catalyst III for reaction, then dropwise adding the rest catalyst III, continuing the heat preservation reaction after dropwise adding to obtain a third intermediate, cooling, adding acrylic acid, stirring and mixing uniformly, dropwise adding catalyst IV, continuing the heat preservation reaction after dropwise adding to obtain a fourth intermediate, cooling, and adjusting the pH value to 5-7 to obtain a metal complexing agent;
(d) preparation of a refining agent: adding the penetrant prepared in the step (a), the hydrogen peroxide low-temperature activator prepared in the step (b), the metal complexing agent prepared in the step (c) and the environment-friendly surfactant into a reaction kettle with water, stirring and mixing uniformly, and adjusting the pH value to 6-8 to obtain the refining agent.
In a refining agent system, a common sulfonic acid type anionic surfactant cannot be used in a system with the concentration of more than 50g/L NaOH; while the nonionic surfactant has a salting-out effect in concentrated alkali, the cloud point and the solubility are greatly reduced, and the two types are not suitable for use. The surfactant adopted in the invention is a carboxylate surfactant, has better alkali resistance and concentrated alkali solubility, and can solve the problems of dissolution and stability of the refining agent.
The low-temperature hydrogen peroxide activation system with the amide structure, which is developed by the invention, does not contain harmful components such as formaldehyde and the like, is basically colorless and odorless, and can be mixed with hydrogen peroxide anions (HOO)-) The reaction generates peroxy acid with strong bleaching ability, so that the refining agent has good oxidation bleaching effect at low temperature. Compared with the European system, the system has the advantages that: 1) the activating agent has better water solubility and is more convenient to use; 2) the activator molecule contains a 9 carbon atom hydrophobic chain, has higher affinity to fabrics and higher activity; 3) the activator has the structure and the property of a surfactant, is beneficial to the permeation of the treatment fluid, and has excellent treatment effect.
The hole-breaking preventing agent used in cold pad-batch scouring and bleaching is mainly used for preventing the formation of holes, avoiding the catalytic decomposition of heavy metal ions and inhibiting the dissociation effect promoted by high alkali. Therefore, the hole-breaking preventing agent used in the cold pad-batch is mainly composed of a chelating agent. The chelating agent is selected to maintain good chelating capacity and high chelating capacity under the condition of high alkali, and a plurality of chelating agents have good chelating capacity at the pH value of 10-11. However, at pH l4, the chelating ability is drastically reduced, and such a chelating agent is not suitable for cold pad-batch bleaching. The chelating agent synthesized by the method has strong capability of chelating heavy metal ions, and is phosphorus-free and environment-friendly.
In the step (a), the mol ratio of the special EO/PO polyether, the fatty ester amine and the maleic anhydride is 1 (1-1.2) to 2, and the adding amount of the catalyst I is 0.05-1% of the total mass of the special EO/PO polyether, the fatty ester amine, the maleic anhydride and the catalyst I.
In the step (a), the reaction temperature for generating the first intermediate is 50-80 ℃, and the reaction time is 4-5 h; the reaction temperature for generating the second intermediate is 60-85 ℃, and the reaction time is 3.5-4 h; the temperature reduction is to be carried out to be below 50 ℃.
In the step (b), the molar ratio of the mixture of the gelatin and the ethylenediamine to the copper sulfate is 1.05-1.1:1, the molar ratio of the gelatin to the ethylenediamine in the mixture of the gelatin and the ethylenediamine is 1:0.95-1, and the dosage of the catalyst II is 5 ppm.
In the step (b), the reaction temperature is kept at 60 ℃ and the reaction time is 3-3.5 h.
In the step (c), the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the dosage of the catalyst III is 5ppm, and the dosage of the catalyst IV is 5 ppm.
In the step (c), the reaction time after the catalyst III of 1/5 is added is 30-40 min; the reaction time for generating the third intermediate is 2-2.5 h; the temperature reduction is to reduce the temperature to 80 ℃; the reaction time for generating the fourth intermediate is 2-2.5 h; the cooling is to below 50 ℃.
In the step (d), the mass ratio of the penetrating agent, the hydrogen peroxide low-temperature activator, the metal complexing agent and the environment-friendly surfactant is 2:1:2: 5; the environment-friendly surfactant is alkyl polyglycoside.
In the step (a), the catalyst I is an alkaline earth metal catalyst; the catalyst II is cobalt tetracarboxyl phthalocyanine; catalyst III is ammonium persulfate, and catalyst IV is sodium persulfate.
The application of the high-efficiency cold pad-batch refining agent is used for a cold pad-batch pretreatment process, and the cold pad-batch pretreatment process comprises the following steps: singeing, pre-padding, scouring and bleaching liquid padding, rolling, rotating and stacking, unwinding and washing, and drying and cropping.
The invention has the beneficial effects that: the synthetic penetrant, the hydrogen peroxide low-temperature activator and the metal complexing agent are designed to be used as main components of the cold pad-batch high-efficiency penetration scouring agent, and the product shows good comprehensive performance through the synergistic effect of the components, not only has the capability of enabling the scouring liquid to quickly penetrate, is resistant to high-concentration alkali liquor (alkali resistance: NaOH 60g/L is less than 15(s); NaOH 200g/L is not floating oil), has good emulsifying dispersion and solubilization capabilities, can be used together with nonionic and anionic products, and enables the hydrogen peroxide to be stable in the high-concentration alkali liquor. It is both penetrant and stabilizer, and is convenient for use, and the scoured and bleached fabric has high capillary effect, high whiteness and low fiber damage.
Drawings
FIG. 1 is a structural view of a reaction vessel of the present invention;
FIG. 2 is an enlarged view taken at A in FIG. 1;
FIG. 3 is a cross-sectional view taken along line B-B of FIG. 1;
FIG. 4 is a graph showing the effect of the refining agent prepared in example 1 of the present invention on the decomposition rate of hydrogen peroxide.
In the figure: the reaction kettle comprises a kettle body 1, a first stirring paddle 2, a second stirring paddle 3, a convex column 31, a barrel part 4, a groove 41, a through groove 42, a first gear disc 5, a disc body 51, a convex tooth 52, a second gear disc 6, a shell 7, a first fixing plate 71, an upper sliding rail 711, a second fixing plate 72, a lower sliding rail 721, a fixing block 73, a gear 8, a motor 81, a driving mechanism 9, a rotating motor 91, a screw rod 92, a connecting rod 93, a mounting block 94, an upper sliding groove 941, a sliding block 95 and a lower sliding groove 951.
Detailed Description
The invention is further described with reference to the accompanying drawings and the detailed description below:
example 1
A preparation method of an efficient cold rolling stack refining agent comprises the following steps:
(a) preparing a high-efficiency penetrating agent: under the protection of nitrogen, mixing special EO/PO polyether, fatty ester amine and an alkaline earth metal catalyst in a reaction kettle, stirring and reacting for 4 hours at 70 ℃ to obtain a first intermediate, adding maleic anhydride, continuing to react for 4 hours at 80 ℃ to obtain a second intermediate, cooling to below 50 ℃, and adjusting the pH to 7 with alkali to obtain the efficient penetrant; wherein the mol ratio of the special EO/PO polyether to the fatty ester amine to the maleic anhydride is 1:1:2, and the adding amount of the alkaline earth metal catalyst is 0.1 percent of the total mass of the special EO/PO polyether to the fatty ester amine to the maleic anhydride to the alkaline earth metal catalyst.
(b) Preparing a hydrogen peroxide low-temperature activating agent: adding a mixture of gelatin and ethylenediamine and copper sulfate into a reaction kettle, heating to 60 ℃, stirring and mixing, adding a tetra-carboxyl cobalt phthalocyanine catalyst at the constant temperature for three times every 2 hours, then carrying out heat preservation reaction at 60 ℃ for 3 hours, and after the reaction is finished, cooling, discharging and purifying to obtain a hydrogen peroxide low-temperature activator; wherein the molar ratio of the mixture of gelatin and ethylenediamine to copper sulfate is 1.05:1, the molar ratio of gelatin to ethylenediamine in the mixture of gelatin and ethylenediamine is 1:1, and the dosage of tetracarboxy cobalt phthalocyanine is 5 ppm.
(c) Preparing a metal complexing agent: dissolving maleic acid and gluconic acid in hot water at 60 ℃ in a third reaction kettle, heating to 95 ℃, adding 1/5 ammonium persulfate catalyst to react for 30min, then dropwise adding the rest ammonium persulfate, controlling the dropwise adding time within 2 hours, continuing to perform heat preservation reaction at 95 ℃ for 2 hours after the dropwise adding is finished to obtain a third intermediate, cooling to 80 ℃, adding acrylic acid, stirring and mixing uniformly, dropwise adding sodium persulfate, controlling the dropwise adding time within 1 hour, continuing to perform heat preservation reaction at 95 ℃ for 2 hours after the dropwise adding is finished to obtain a fourth intermediate, cooling to below 50 ℃, adjusting the neutralization to pH value of 7 with liquid alkali to obtain a metal complexing agent; wherein the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the dosage of the ammonium persulfate is 5ppm, and the dosage of the sodium persulfate is 5 ppm. When the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the synthesized terpolymer has the strongest chelating and dispersing capacity, and can play a good synergistic role when being applied to the cold pad-batch pretreatment auxiliary agent.
(d) Preparation of a refining agent: adding the penetrant prepared in the step (a), the hydrogen peroxide low-temperature activator prepared in the step (b), the metal complexing agent prepared in the step (c) and the environment-friendly surfactant into a reaction kettle with water, stirring and mixing uniformly, and adjusting the pH value to 7 to obtain a refining agent; wherein the mass ratio of the penetrating agent to the hydrogen peroxide low-temperature activator to the metal complexing agent to the environment-friendly surfactant is 2:1:2: 5; the environment-friendly surfactant is alkyl polyglycoside.
Example 2
A preparation method of an efficient cold rolling stack refining agent comprises the following steps:
(a) preparing a high-efficiency penetrating agent: under the protection of nitrogen, mixing special EO/PO polyether, fatty ester amine and an alkaline earth metal catalyst in a reaction kettle, stirring and reacting for 5 hours at 50 ℃ to obtain a first intermediate, adding maleic anhydride, continuing to react for 4 hours at 65 ℃ to obtain a second intermediate, then cooling to below 50 ℃, and adjusting the pH to 6 with alkali to obtain the efficient penetrant; wherein the mol ratio of the special EO/PO polyether to the fatty ester amine to the maleic anhydride is 1:1.2:2, and the adding amount of the alkaline earth metal catalyst is 0.3 percent of the total mass of the special EO/PO polyether to the fatty ester amine to the maleic anhydride to the alkaline earth metal catalyst.
(b) Preparing a hydrogen peroxide low-temperature activating agent: adding a mixture of gelatin and ethylenediamine and copper sulfate into a reaction kettle, heating to 60 ℃, stirring and mixing, adding a tetra-carboxyl cobalt phthalocyanine catalyst at the constant temperature for three times every 2 hours, then carrying out heat preservation reaction at 60 ℃ for 3.5 hours, and after the reaction is finished, cooling, discharging and purifying to obtain a hydrogen peroxide low-temperature activator; wherein the molar ratio of the mixture of gelatin and ethylenediamine to copper sulfate is 1.08:1, the molar ratio of gelatin to ethylenediamine in the mixture of gelatin and ethylenediamine is 1:1, and the dosage of the tetracarboxy cobalt phthalocyanine is 5 ppm.
(c) Preparing a metal complexing agent: dissolving maleic acid and gluconic acid in hot water at 60 ℃ in a third reaction kettle, heating to 98 ℃, adding 1/5 ammonium persulfate catalyst to react for 40min, then dropwise adding the rest ammonium persulfate, controlling the dropwise adding time within 2 hours, continuing to perform heat preservation reaction at 98 ℃ for 2 hours after the dropwise adding is finished to obtain a third intermediate, cooling to 80 ℃, adding acrylic acid, stirring and mixing uniformly, dropwise adding sodium persulfate, controlling the dropwise adding time within 1 hour, continuing to perform heat preservation reaction at 98 ℃ for 2 hours after the dropwise adding is finished to obtain a fourth intermediate, cooling to below 50 ℃, adjusting the neutralization to pH value of 5 with liquid alkali to obtain a metal complexing agent; wherein the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the dosage of the ammonium persulfate is 5ppm, and the dosage of the sodium persulfate is 5 ppm. When the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the synthesized terpolymer has the strongest chelating and dispersing capacity, and can play a good synergistic role when being applied to the cold pad-batch pretreatment auxiliary agent.
(d) Preparation of a refining agent: adding the penetrant prepared in the step (a), the hydrogen peroxide low-temperature activator prepared in the step (b), the metal complexing agent prepared in the step (c) and the environment-friendly surfactant into a reaction kettle with water, stirring and mixing uniformly, and adjusting the pH value to 6 to obtain a refining agent; wherein the mass ratio of the penetrating agent to the hydrogen peroxide low-temperature activator to the metal complexing agent to the environment-friendly surfactant is 2:1:2: 5; the environment-friendly surfactant is alkyl polyglycoside.
Example 3
A preparation method of an efficient cold rolling stack refining agent comprises the following steps:
(a) preparing a high-efficiency penetrating agent: under the protection of nitrogen, mixing special EO/PO polyether, fatty ester amine and an alkaline earth metal catalyst in a reaction kettle, stirring and reacting for 4 hours at 80 ℃ to obtain a first intermediate, adding maleic anhydride, continuing to react for 3.5 hours at 85 ℃ to obtain a second intermediate, cooling to below 50 ℃, and adjusting the pH to 8 by using alkali to obtain a high-efficiency penetrating agent; wherein the mol ratio of the special EO/PO polyether to the fatty ester amine to the maleic anhydride is 1:1.1:2, and the addition amount of the alkaline earth metal catalyst is 0.5 percent of the total mass of the special EO/PO polyether to the fatty ester amine to the maleic anhydride to the alkaline earth metal catalyst.
(b) Preparing a hydrogen peroxide low-temperature activating agent: adding a mixture of gelatin and ethylenediamine and copper sulfate into a reaction kettle, heating to 60 ℃, stirring and mixing, adding a tetra-carboxyl cobalt phthalocyanine catalyst at the constant temperature for three times every 2 hours, then carrying out heat preservation reaction at 60 ℃ for 3 hours, and after the reaction is finished, cooling, discharging and purifying to obtain a hydrogen peroxide low-temperature activator; wherein the molar ratio of the mixture of gelatin and ethylenediamine to copper sulfate is 1.1:1, the molar ratio of gelatin to ethylenediamine in the mixture of gelatin and ethylenediamine is 1:0.95, and the dosage of the cobalt tetracarboxy phthalocyanine is 5 ppm.
(c) Preparing a metal complexing agent: dissolving maleic acid and gluconic acid in hot water at 60 ℃ in a third reaction kettle, heating to 96 ℃, adding 1/5 ammonium persulfate catalyst to react for 30min, then dropwise adding the rest ammonium persulfate, controlling the dropwise adding time within 2 hours, continuing to perform heat preservation reaction at 96 ℃ for 2 hours after the dropwise adding is finished to obtain a third intermediate, cooling to 80 ℃, adding acrylic acid, stirring and mixing uniformly, dropwise adding sodium persulfate, controlling the dropwise adding time within 1 hour, continuing to perform heat preservation reaction at 96 ℃ for 2 hours after the dropwise adding is finished to obtain a fourth intermediate, cooling to below 50 ℃, adjusting the neutralization to pH value of 7 with liquid alkali to obtain a metal complexing agent; wherein the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the dosage of the ammonium persulfate is 5ppm, and the dosage of the sodium persulfate is 5 ppm. When the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the synthesized terpolymer has the strongest chelating and dispersing capacity, and can play a good synergistic role when being applied to the cold pad-batch pretreatment auxiliary agent.
(d) Preparation of a refining agent: adding the penetrant prepared in the step (a), the hydrogen peroxide low-temperature activator prepared in the step (b), the metal complexing agent prepared in the step (c) and the environment-friendly surfactant into a reaction kettle with water, stirring and mixing uniformly, and adjusting the pH value to 8 to obtain a refining agent; wherein the mass ratio of the penetrating agent to the hydrogen peroxide low-temperature activator to the metal complexing agent to the environment-friendly surfactant is 2:1:2: 5; the environment-friendly surfactant is alkyl polyglycoside.
Example 4
A preparation method of an efficient cold rolling stack refining agent comprises the following steps:
(a) preparing a high-efficiency penetrating agent: under the protection of nitrogen, mixing special EO/PO polyether, fatty ester amine and an alkaline earth metal catalyst in a reaction kettle, stirring and reacting for 4 hours at 60 ℃ to obtain a first intermediate, adding maleic anhydride, continuing to react for 4 hours at 75 ℃ to obtain a second intermediate, cooling to below 50 ℃, and adjusting the pH to 7 with alkali to obtain the efficient penetrant; wherein the mol ratio of the special EO/PO polyether to the fatty ester amine to the maleic anhydride is 1:1.1:2, and the adding amount of the alkaline earth metal catalyst is 0.05 percent of the total mass of the special EO/PO polyether to the fatty ester amine to the maleic anhydride to the alkaline earth metal catalyst.
(b) Preparing a hydrogen peroxide low-temperature activating agent: adding a mixture of gelatin and ethylenediamine and copper sulfate into a reaction kettle, heating to 60 ℃, stirring and mixing, adding a tetra-carboxyl cobalt phthalocyanine catalyst at the constant temperature for three times every 2 hours, then carrying out heat preservation reaction at 60 ℃ for 3.5 hours, and after the reaction is finished, cooling, discharging and purifying to obtain a hydrogen peroxide low-temperature activator; wherein the molar ratio of the mixture of gelatin and ethylenediamine to copper sulfate is 1:1, the molar ratio of gelatin to ethylenediamine in the mixture of gelatin and ethylenediamine is 1:0.95, and the dosage of tetracarboxy cobalt phthalocyanine is 5 ppm.
(c) Preparing a metal complexing agent: dissolving maleic acid and gluconic acid in hot water at 60 ℃ in a third reaction kettle, heating to 95 ℃, adding 1/5 ammonium persulfate catalyst to react for 40min, then dropwise adding the rest ammonium persulfate, controlling the dropwise adding time within 2 hours, continuing to perform heat preservation reaction at 95 ℃ for 2.5 hours after dropwise adding to obtain a third intermediate, cooling to 80 ℃, adding acrylic acid, stirring and mixing uniformly, dropwise adding sodium persulfate, controlling the dropwise adding time within 1 hour, continuing to perform heat preservation reaction at 95 ℃ for 2.5 hours after dropwise adding to obtain a fourth intermediate, cooling to below 50 ℃, adjusting the neutralization to pH value of 6 with liquid alkali to obtain a metal complexing agent; wherein the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the dosage of the ammonium persulfate is 5ppm, and the dosage of the sodium persulfate is 5 ppm. When the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the synthesized terpolymer has the strongest chelating and dispersing capacity, and can play a good synergistic role when being applied to the cold pad-batch pretreatment auxiliary agent.
(d) Preparation of a refining agent: adding the penetrant prepared in the step (a), the hydrogen peroxide low-temperature activator prepared in the step (b), the metal complexing agent prepared in the step (c) and the environment-friendly surfactant into a reaction kettle with water, stirring and mixing uniformly, and adjusting the pH value to 7 to obtain a refining agent; wherein the mass ratio of the penetrating agent to the hydrogen peroxide low-temperature activator to the metal complexing agent to the environment-friendly surfactant is 2:1:2: 5; the environment-friendly surfactant is alkyl polyglycoside.
Example 5
A preparation method of an efficient cold rolling stack refining agent comprises the following steps:
(a) preparing a high-efficiency penetrating agent: under the protection of nitrogen, mixing special EO/PO polyether, fatty ester amine and an alkaline earth metal catalyst in a reaction kettle, stirring and reacting for 4 hours at 60 ℃ to obtain a first intermediate, adding maleic anhydride, continuing to react for 4 hours at 80 ℃ to obtain a second intermediate, cooling to below 50 ℃, and adjusting the pH to 8 by using alkali to obtain the efficient penetrant; wherein the mol ratio of the special EO/PO polyether to the fatty ester amine to the maleic anhydride is 1:1:2, and the adding amount of the alkaline earth metal catalyst is 1 percent of the total mass of the special EO/PO polyether to the fatty ester amine to the maleic anhydride to the alkaline earth metal catalyst.
(b) Preparing a hydrogen peroxide low-temperature activating agent: adding a mixture of gelatin and ethylenediamine and copper sulfate into a reaction kettle, heating to 60 ℃, stirring and mixing, adding a tetra-carboxyl cobalt phthalocyanine catalyst at the constant temperature for three times every 2 hours, then carrying out heat preservation reaction at 60 ℃ for 3.5 hours, and after the reaction is finished, cooling, discharging and purifying to obtain a hydrogen peroxide low-temperature activator; wherein the molar ratio of the mixture of gelatin and ethylenediamine to copper sulfate is 1.07:1, the molar ratio of gelatin to ethylenediamine in the mixture of gelatin and ethylenediamine is 1:1, and the dosage of tetracarboxy cobalt phthalocyanine is 5 ppm.
(c) Preparing a metal complexing agent: dissolving maleic acid and gluconic acid in hot water at 60 ℃ in a third reaction kettle, heating to 95 ℃, adding 1/5 ammonium persulfate catalyst to react for 30min, then dropwise adding the rest ammonium persulfate, controlling the dropwise adding time within 2 hours, continuing to perform heat preservation reaction at 95 ℃ for 2 hours after the dropwise adding is finished to obtain a third intermediate, cooling to 80 ℃, adding acrylic acid, stirring and mixing uniformly, dropwise adding sodium persulfate, controlling the dropwise adding time within 1 hour, continuing to perform heat preservation reaction at 95 ℃ for 2 hours after the dropwise adding is finished to obtain a fourth intermediate, cooling to below 50 ℃, adjusting the neutralization to pH value to 6 with liquid alkali to obtain a metal complexing agent; wherein the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the dosage of the ammonium persulfate is 5ppm, and the dosage of the sodium persulfate is 5 ppm. When the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the synthesized terpolymer has the strongest chelating and dispersing capacity, and can play a good synergistic role when being applied to the cold pad-batch pretreatment auxiliary agent.
(d) Preparation of a refining agent: adding the penetrant prepared in the step (a), the hydrogen peroxide low-temperature activator prepared in the step (b), the metal complexing agent prepared in the step (c) and the environment-friendly surfactant into a reaction kettle with water, stirring and mixing uniformly, and adjusting the pH value to 7 to obtain a refining agent; wherein the mass ratio of the penetrating agent to the hydrogen peroxide low-temperature activator to the metal complexing agent to the environment-friendly surfactant is 2:1:2: 5; the environment-friendly surfactant is alkyl polyglycoside.
The reaction kettle is designed according to different technological conditions and needs to realize the heating, evaporating, cooling and low-speed mixing reaction functions required by the technology. Present reation kettle agitating unit is comparatively simple, can only carry out single direction mixing stirring, and stirring effect is not good, and the temperature is different easily appearing in the upper and lower part in the reation kettle to cause the upper and lower part liquid mixing reaction degree in the reation kettle to differ, lead to mixed liquid quality inhomogeneous.
In the steps of the embodiment of the invention, reaction kettles with the same structure are adopted, as shown in fig. 1-3, the reaction kettle comprises a kettle body 1 and a stirring device extending into the kettle body 1, the stirring device comprises a first stirring paddle 2, a second stirring paddle 3, a barrel 4, a first gear plate 5 and a second gear plate 6 which are arranged above the kettle body 1 and are arranged oppositely up and down, the first gear plate 5 and the second gear plate 6 can rotate simultaneously and rotate in opposite directions, the first stirring paddle 2 is fixed on the first gear plate 5, the first stirring paddle 2 penetrates through the second gear plate 6 and then extends into the kettle body 1, the first stirring paddle 2 is driven to rotate by the first gear plate 5, one end of the barrel 4 is fixedly connected to the second gear plate 6, the other end of the barrel 4 is rotatably connected with the top of the kettle body 1, the second stirring paddle 3 is arranged between the first stirring paddle 2 and the barrel 4, shaft part and 4 circumference spacing connections of section of thick bamboo spares of second stirring rake 3 and second stirring rake 3 can follow section of thick bamboo spares 4 up-and-down motion and fix a position to required height, second stirring rake 3 passes through 6 drive rotations of second gear disc.
The first gear disc 5 and the second gear disc 6 are driven by a pair of symmetrically arranged gears 8 to do opposite rotation movement, and the gears 8 are driven to rotate by a motor 81.
1 top of the cauldron body is fixed with casing 7, first toothed disc 5 and second toothed disc 6 set up in casing 7, first toothed disc 5 and second toothed disc 6 all include disk body 51 and the dogtooth 52 that distributes by the protruding circumference that forms in disk body 51 surface, the dogtooth 52 of first toothed disc 5 and second toothed disc 6 sets up for relative. The pair of gears 8 are symmetrically arranged by taking the shaft of the first stirring paddle 2 as a center, the convex teeth 52 of the first gear disc 5 and the convex teeth 52 of the second gear disc 6 are meshed with the pair of gears 8 at the same time, and when the two gears 8 rotate, the first gear disc 5 and the second gear disc 6 can be driven to do opposite rotation motion.
Leave the clearance between the axial region of first stirring rake 2 and the second gear wheel dish 6, the axial region laminating of the axial region of first stirring rake 2 and second stirring rake 3 rotates the setting to guarantee the relative antiport of first stirring rake 2 and second stirring rake 3. The axial region of first stirring rake 2 and the axial region coating polyethylene coating of second stirring rake 3, pass through the sealing washer between the axial region lower extreme of second stirring rake 3 and the axial region of first stirring rake 2 and seal.
Second stirring rake 3 and 4 circumference limit structure of section of thick bamboo spare are: the outer wall of the shaft part of the second stirring paddle 3 is protruded to form a plurality of pairs of convex columns 31, and the annular inner wall of the barrel part 4 is sunken to form a plurality of pairs of concave columns 31 which are correspondingly clamped into grooves 41.
The second stirring paddle 3 is driven by the driving mechanism 9 to move up and down and position, and the second stirring paddle 3 drives the driving mechanism 9 to rotate concentrically.
A through groove 42 is formed in one side of the barrel 4, and the connecting rod 93 penetrates through the through groove 42 and can slide along the through groove 42.
The mounting block 94 is provided with an upper concave surface forming an upper sliding groove 941, and the lower surface of the first fixing plate 71 is protruded to form an annular upper sliding rail 711 slidably engaged with the upper sliding groove 941. The upper surface of the second fixing plate 72 is provided with an annular lower slide rail 721, and the lower surface of the slider 95 is provided with a lower slide groove 951 which is slidably engaged with the lower slide rail 721.
Fixed block 73 is fixed on the top of casing 7, first stirring rake 2 rotates with fixed block 73 and is connected.
According to the reaction kettle, the first stirring paddle 2 is driven to rotate by the first gear disc 5, the barrel part 4 is driven to rotate by the second gear disc 6, and then the second stirring paddle 3 is driven to rotate, so that the first stirring paddle 2 and the second stirring paddle 3 can rotate in different directions simultaneously, the height of the paddle of the second stirring paddle 3 is adjustable, the stirring position of the second stirring paddle 3 can be adjusted according to the liquid level height, the second stirring paddle 3 can move up and down while stirring, the stirring effect is further improved, and the stirring uniformity is improved.
The performance tests (including fabric whiteness, fabric capillary, fabric strength, and fabric alkali resistance permeability) of the refining agents prepared in examples 1 to 5 were performed, and the results are shown in tables 1 to 4, using a commercially available refining agent A produced in a certain country and a refining agent B imported from a certain country as a comparison.
TABLE 1 Effect of different amounts of scouring Agents on Fabric whiteness
As can be seen from Table 1, the whiteness of the fabric prepared by using the refining agent provided by the invention is higher under the same dosage, the whiteness of the fabric is obviously increased between 5g/L and 10g/L along with the increase of the dosage of the refining agent, mainly impurities such as cottonseed hulls and ash on cotton yarns react with the refining agent to become water-soluble substances which are dissolved in water, slurry falls off under the strong permeability of the refining agent and is dissolved in the water, and pigment is mainly formed by H2O2And the oxidation generates decoloration, thereby improving the whiteness of the fabric. The whiteness of the fabric with 15g/L of scouring agent is close to that of the fabric with 10g/L, the difference is not more than 1%, and the whiteness is not obviously improved when the dosage of the scouring agent reaches 20 g/L.
TABLE 2 Effect of different amounts of scouring agent on Hair Effect
From the table 2 and can be seen, the wool effect of the fabric is obviously increased along with the increase of the dosage of the scouring agent, and mainly, impurities such as grease wax on cotton yarns react with the scouring agent under the action of strong caustic soda to become water-soluble substances which are dissolved in water, so that the water absorption performance of the fabric is improved, and the wool effect is greatly improved. Compared with various refining agents, the refining agent prepared by the invention has the performance close to that of the imported refining agent B, and the capillary effect can reach 12.
TABLE 3 Effect of different amounts of scouring Agents on Fabric Strength
It is understood from Table 3 that the strength is not greatly affected by changing the concentration of the scouring agent when the concentration of the hydrogen peroxide and the oxygen bleaching stabilizer is not changed. The strength values of the tested products are over 600N, so that the damage to the strength caused by cold pad-batch pretreatment is small.
TABLE 4 alkali penetration resistance of the respective scouring Agents
As is clear from Table 4, the refining agent prepared by the present invention is the most resistant to alkali at a high concentration of caustic soda.
The alkali resistance of the scouring agent directly affects the usability of the scouring agent in factories which generally use 1:3 concentrations for batching, so the alkali resistance becomes an important index. The conventional requirement reaches more than 150 g/L.
The effect of the refining agent and the commercially available oxygen bleaching stabilizer 815 prepared in example 1 of the present invention on the decomposition rate of hydrogen peroxide is shown in fig. 4. As can be seen from figure 4, the refining agent has an obvious stabilizing effect on hydrogen peroxide, and the decomposition rate of the hydrogen peroxide cannot be reduced along with the prolonging of time, so that the scouring and bleaching effect is ensured, because the metal chelating agent in the refining agent has the effect of the oxygen bleaching stabilizer, metal ions in the working solution can be effectively complexed, the decomposition rate of the hydrogen peroxide is controlled, and the refining agent has a good hydrogen peroxide activation effect.
The application of the high-efficiency cold pad-batch refining agent is used for a cold pad-batch pretreatment process, and the cold pad-batch pretreatment process comprises the following steps: singeing, pre-padding (room temperature and mangling allowance of 80 percent), scouring and bleaching liquid padding (room temperature and mangling allowance of 100 to 110 percent), rolling, rotating and stacking (covering with a plastic film, moisturizing, rotating and stacking for 24 hours), uncoiling, washing with water (hot water washing, hot alkali washing, hot water washing and water washing), and drying and cropping.
The refining agent prepared in the embodiment 1 is applied to a cold pad-batch pretreatment process and a treatment effect is tested, and the process formula is as follows: NaOH 40-60g/L, hydrogen peroxide 20g/L, scouring agent 15g/L, the results are shown in Table 5.
TABLE 5
| Classes of fabrics | Hair effect (cm) | Whiteness (%) | Cotton seed husk removal |
| Yarn card (old art) | 12.2 | 74 | Good effect |
| Yarn card | 13.3 | 77 | Good effect |
| Poplin | 14.1 | 76 | Good effect |
| High-density poplin | 12.8 | 74 | Good effect |
As can be seen from Table 5, the high-efficiency scouring agent prepared by the invention can achieve better capillary effect and whiteness in cold pad batch refining application.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A preparation method of an efficient cold rolling batch refining agent is characterized by comprising the following steps: the method comprises the following steps:
(a) preparing a high-efficiency penetrating agent: under the protection of nitrogen, mixing and stirring the special EO/PO polyether, the fatty ester amine and the catalyst I in a reaction kettle to react to obtain a first intermediate, adding maleic anhydride to continue the reaction to obtain a second intermediate, and cooling and adjusting the pH value to 6-8 to obtain the high-efficiency penetrating agent;
(b) preparing a hydrogen peroxide low-temperature activating agent: adding a mixture of gelatin and ethylenediamine and copper sulfate into a reaction kettle, heating to 60 ℃, stirring and mixing, adding a catalyst II at the constant temperature for three times every 2 hours, then carrying out heat preservation reaction, and after the reaction is finished, cooling, discharging and purifying to obtain a hydrogen peroxide low-temperature activator;
(c) preparing a metal complexing agent: dissolving maleic acid and gluconic acid in hot water in a third reaction kettle, heating to 95-98 ℃, adding 1/5 catalyst III for reaction, then dropwise adding the rest catalyst III, continuing the heat preservation reaction after dropwise adding to obtain a third intermediate, cooling, adding acrylic acid, stirring and mixing uniformly, dropwise adding catalyst IV, continuing the heat preservation reaction after dropwise adding to obtain a fourth intermediate, cooling, and adjusting the pH value to 5-7 to obtain a metal complexing agent;
(d) preparation of a refining agent: adding the penetrant prepared in the step (a), the hydrogen peroxide low-temperature activator prepared in the step (b), the metal complexing agent prepared in the step (c) and the environment-friendly surfactant into a reaction kettle with water, stirring and mixing uniformly, and adjusting the pH value to 6-8 to obtain the refining agent.
2. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (a), the mol ratio of the special EO/PO polyether, the fatty ester amine and the maleic anhydride is 1 (1-1.2) to 2, and the adding amount of the catalyst I is 0.05-1% of the total mass of the special EO/PO polyether, the fatty ester amine, the maleic anhydride and the catalyst I.
3. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (a), the reaction temperature for generating the first intermediate is 50-80 ℃, and the reaction time is 4-5 h; the reaction temperature for generating the second intermediate is 60-85 ℃, and the reaction time is 3.5-4 h; the temperature reduction is to be carried out to be below 50 ℃.
4. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (b), the molar ratio of the mixture of the gelatin and the ethylenediamine to the copper sulfate is 1.05-1.1:1, the molar ratio of the gelatin to the ethylenediamine in the mixture of the gelatin and the ethylenediamine is 1:0.95-1, and the dosage of the catalyst II is 5 ppm.
5. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (b), the reaction temperature is kept at 60 ℃ and the reaction time is 3-3.5 h.
6. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (c), the molar ratio of the maleic acid to the gluconic acid to the acrylic acid is 1:1.5:0.5, the dosage of the catalyst III is 5ppm, and the dosage of the catalyst IV is 5 ppm.
7. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (c), the reaction time after the catalyst III of 1/5 is added is 30-40 min; the reaction time for generating the third intermediate is 2-2.5 h; the temperature reduction is to reduce the temperature to 80 ℃; the reaction time for generating the fourth intermediate is 2-2.5 h; the cooling is to below 50 ℃.
8. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (d), the mass ratio of the penetrating agent, the hydrogen peroxide low-temperature activator, the metal complexing agent and the environment-friendly surfactant is 2:1:2: 5; the environment-friendly surfactant is alkyl polyglycoside.
9. The method for preparing the high-efficiency cold rolling batch refining agent as claimed in claim 1, wherein the method comprises the following steps: in the step (a), the catalyst I is an alkaline earth metal catalyst; the catalyst II is cobalt tetracarboxyl phthalocyanine; catalyst III is ammonium persulfate, and catalyst IV is sodium persulfate.
10. Use of a high-performance cold roll stack refining agent prepared according to the method of any one of claims 1 to 9, characterized in that: the scouring agent is used for a cold pad-batch pretreatment process, and the cold pad-batch pretreatment process comprises the following steps: singeing, pre-padding, scouring and bleaching liquid padding, rolling, rotating and stacking, unwinding and washing, and drying and cropping.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114875654A (en) * | 2022-06-10 | 2022-08-09 | 山东中康国创先进印染技术研究院有限公司 | Low-strength-loss cold pad-batch pretreatment process for desizing, scouring and bleaching of cotton fabrics |
| CN117563543A (en) * | 2024-01-15 | 2024-02-20 | 扬州伟毅通用设备有限公司 | Circulation stirring formula chemical industry equipment reation kettle |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440572A (en) * | 2008-12-29 | 2009-05-27 | 邵国标 | Environment protection type alkaliproof refining agent and preparation thereof |
| CN104594012A (en) * | 2013-10-30 | 2015-05-06 | 青岛鑫益发工贸有限公司 | Low-temperature scouring and bleaching method for pure cotton fabric |
| CN104611906A (en) * | 2015-01-14 | 2015-05-13 | 西安工程大学 | Hydrogen peroxide bleaching catalyst and preparation method thereof |
| CN111675792A (en) * | 2020-06-28 | 2020-09-18 | 广东传化富联精细化工有限公司 | Multifunctional chelating dispersion protective colloid for fabric and preparation method thereof |
-
2021
- 2021-07-28 CN CN202110855634.5A patent/CN113564912A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440572A (en) * | 2008-12-29 | 2009-05-27 | 邵国标 | Environment protection type alkaliproof refining agent and preparation thereof |
| CN104594012A (en) * | 2013-10-30 | 2015-05-06 | 青岛鑫益发工贸有限公司 | Low-temperature scouring and bleaching method for pure cotton fabric |
| CN104611906A (en) * | 2015-01-14 | 2015-05-13 | 西安工程大学 | Hydrogen peroxide bleaching catalyst and preparation method thereof |
| CN111675792A (en) * | 2020-06-28 | 2020-09-18 | 广东传化富联精细化工有限公司 | Multifunctional chelating dispersion protective colloid for fabric and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 金黔宏等: "高效冷轧堆精练剂ZL-321的研制和应用", 《全国印染助剂行业研讨会暨江苏省印染助剂情报站第25届年会论文集》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114875654A (en) * | 2022-06-10 | 2022-08-09 | 山东中康国创先进印染技术研究院有限公司 | Low-strength-loss cold pad-batch pretreatment process for desizing, scouring and bleaching of cotton fabrics |
| CN114875654B (en) * | 2022-06-10 | 2023-11-21 | 山东中康国创先进印染技术研究院有限公司 | Pretreatment process for desizing, boiling and bleaching low-strength-loss cold pad-batch of cotton fabric |
| CN117563543A (en) * | 2024-01-15 | 2024-02-20 | 扬州伟毅通用设备有限公司 | Circulation stirring formula chemical industry equipment reation kettle |
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Application publication date: 20211029 |