CN114541145A - Application of organic silicon emulsion hand feeling deepening finishing agent - Google Patents
Application of organic silicon emulsion hand feeling deepening finishing agent Download PDFInfo
- Publication number
- CN114541145A CN114541145A CN202210142659.5A CN202210142659A CN114541145A CN 114541145 A CN114541145 A CN 114541145A CN 202210142659 A CN202210142659 A CN 202210142659A CN 114541145 A CN114541145 A CN 114541145A
- Authority
- CN
- China
- Prior art keywords
- organic silicon
- hand feeling
- finishing agent
- comb
- silicone oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 50
- 239000010703 silicon Substances 0.000 title claims abstract description 50
- 239000000839 emulsion Substances 0.000 title claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 30
- 229920002545 silicone oil Polymers 0.000 claims abstract description 38
- 230000000694 effects Effects 0.000 claims abstract description 11
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 19
- 229920002554 vinyl polymer Polymers 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 230000009471 action Effects 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000004945 emulsification Methods 0.000 claims description 8
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 claims description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- PELGKMTVNFFDDL-UHFFFAOYSA-N dodecyl-dimethoxy-methylsilane Chemical compound CCCCCCCCCCCC[Si](C)(OC)OC PELGKMTVNFFDDL-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000009998 heat setting Methods 0.000 claims description 7
- 238000009775 high-speed stirring Methods 0.000 claims description 7
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 230000006837 decompression Effects 0.000 claims description 5
- 239000000675 fabric finishing Substances 0.000 claims description 3
- 238000009962 finishing (textile) Methods 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 239000004744 fabric Substances 0.000 abstract description 21
- 239000010408 film Substances 0.000 abstract description 7
- 125000005358 mercaptoalkyl group Chemical group 0.000 abstract description 7
- 230000009257 reactivity Effects 0.000 abstract description 6
- 150000001335 aliphatic alkanes Chemical group 0.000 abstract description 5
- 125000004103 aminoalkyl group Chemical group 0.000 abstract description 4
- 239000000835 fiber Substances 0.000 abstract description 3
- 238000012650 click reaction Methods 0.000 abstract description 2
- 239000013039 cover film Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000007822 coupling agent Substances 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- 239000012224 working solution Substances 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- -1 acrylic ester Chemical class 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229920013822 aminosilicone Polymers 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000002653 sulfanylmethyl group Chemical group [H]SC([H])([H])[*] 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Classifications
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
-
- 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 an application of an organosilicon emulsion darkening hand feeling finishing agent, and synthesizes comb-shaped organosilicon containing long-chain alkane, mercaptoalkyl and aminoalkyl side chains, which has reactivity and a function of covering a film on the surface to increase diffuse reflection. Because the organosilicon main chain has low refractive index and contains amino alkyl, the affinity with the fabric is strong, and long-chain alkane enables the finishing agent to form a film, the concave-convex performance of the fabric surface is improved, the diffuse reflection is increased, and a concave-convex low-refractive-index film can be formed on the fiber surface. Through introducing a mercapto-alkyl group with reactivity into an organic silicon side chain, the reactivity of the mercapto-alkyl group with vinyl-terminated silicone oil is improved based on a mercapto-alkene click reaction, and a branched organic silicon emulsion is formed. When the fabric is finished, the complexity of the cloth cover film is improved by constructing the branched structure, and the deepening effect of the product is further improved.
Description
Technical Field
The invention belongs to the field of textile printing and dyeing processing and after finishing, and particularly relates to an application of an organic silicon emulsion hand feeling enhancing finishing agent.
Background
At present, as the traditional strut industry in China, namely textile industry, a great deal of dye consumption in the printing and dyeing process and a great deal of waste water generation bring heavy burden to the environment and resources. With the rapid rectification of the printing and dyeing industry, the strict monitoring of non-environment-friendly dyes, energy conservation, emission reduction and technical transformation of the non-environment-friendly dyes in recent years, the improvement of the product competitiveness becomes an urgent task of the industry. In addition, with the popularization of novel superfine fiber fabrics, the problem of fabric dyeing depth is increasingly emphasized. By adopting the deepening technology, the dye can be saved, the wastewater discharge can be reduced, and the problem of deep color effect which cannot be achieved by increasing the dye dosage can be solved.
Currently, polyurethane resin finishing agents, acrylic resin finishing agents, organic fluorine finishing agents and organic silicon finishing agents are used in the market.
The first three products have no smoothness basically after finishing due to structural limitation, and the wearability is not high, so that the fabric treated by the three deepened products still needs to be subjected to organosilicon hand feeling finishing again in the after-finishing stage. After the acrylic ester product is used for treating the fabric, the fabric is extremely rough, poor in elasticity and surface finish, and the fluorine-containing raw material of the organic fluorine finishing agent also has the problems of economy, environmental protection and the like.
Because the organic silicon oxygen bond has rotation property, the organic silicon oxygen bond is easy to permeate oxygen, nitrogen and the like, the treated fabric has soft and fluffy performance and good smooth feeling, and the organic silicon oxygen bond is widely used in the fabric after-finishing stage, but the conventional organic silicon hand feeling finishing agent such as amino silicone oil and block silicone oil can not achieve ideal deepening effect generally.
Disclosure of Invention
The invention aims to provide the application of the cheap and good organic silicon emulsion deepening hand feeling finishing agent which is simple and reasonable in structure, easy to clean and maintain and overcomes the defects of the prior art.
The technical scheme for solving the technical problem is as follows: an application of an organosilicon emulsion deepening hand feeling finishing agent, the organosilicon emulsion deepening hand feeling finishing agent has the following structure:
the preparation method of the organic silicon emulsion darkening hand feeling finishing agent comprises the following steps: 1) preparing comb-shaped organic silicon: linear body, dodecyl methyl dimethoxy silane, mercaptopropyl methyl dimethoxy silane and N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane are adopted as raw materials, and are subjected to prepolymerization reaction for 0.5-4 h and vacuum decompression reaction for 1-10 h under the action of an alkaline catalyst, so that the comb-shaped silicone oil with high affinity, soft hand feeling and good deepening effect is obtained; 2) preparation of branched silicone emulsion: adding comb-shaped organic silicon into a four-neck flask with a thermometer, heating to 50-70 ℃, adding vinyl silicone oil step by step under the action of a triethanolamine catalyst, and stirring for reaction for 30 minutes to 2 hours to obtain organic silicone oil with a branched structure; adding a surfactant, and adding deionized water under high-speed stirring for emulsification and dispersion to obtain the branched-structure organic silicon emulsion.
The application of the organic silicon emulsion darkening hand feeling finishing agent comprises the following steps: the organic silicon emulsion deepening hand feeling finishing agent is applied to fabric finishing, the concentration of the finishing liquid of the organic silicon emulsion deepening hand feeling finishing agent is not less than 20g/L, and the application process is as follows: one-dipping and one-rolling, drying at 100 ℃, and heat setting at 150-180 ℃ for 90 s.
The beneficial effects of the invention are:
the comb-type organic silicon with a specific main chain is generated by controlling the reaction ratio of the ammonia-hydrocarbon-based coupling agent, the mercapto-hydrocarbon-based coupling agent, the long-chain alkane coupling agent and the linear body, the design of the molecular weight of the silicone oil and the selection of an emulsification process. In order to further improve the deepening effect of the finishing agent on the fabric, vinyl silicone oil and comb-shaped organic silicon are introduced to react to synthesize branched organic silicon, the formula of the finishing agent is optimized, and the deepening effect, the hand feeling and other properties of the finished fabric are examined.
The invention designs and synthesizes comb-shaped organic silicon containing long-chain alkane, mercaptoalkyl and aminoalkyl side chains, which has reactivity and a function of increasing diffuse reflection by coating a film on the surface. Because the organosilicon main chain has low refractive index and amino-hydrocarbon group, and has strong affinity with the fabric, the long-chain alkane increases the concave-convex performance of the fabric surface after the finishing agent is formed into a film, increases diffuse reflection, and can form a concave-convex low-refractive-index film on the fiber surface. The method is characterized in that a mercapto-alkyl group with reactivity is introduced into an organic silicon side chain, and the reactivity of the mercapto-alkyl group with vinyl-terminated silicone oil is improved based on a mercapto-alkene click reaction, so that a branched organic silicon emulsion is formed. When the fabric is finished, the complexity of the cloth cover film is improved by constructing the branched structure, and the deepening effect of the product is further improved.
The organic silicon fabric deepening hand feeling finishing agent obtained by the invention not only keeps the excellent smooth hand feeling of organic silicon, but also obtains an excellent deepening effect, can reduce the deepening treatment of the working procedures before fabric finishing, is economic and environment-friendly, and has very high commercial value.
In conclusion, the invention has the advantages of easily obtained raw materials, simple preparation process, low industrialization cost and low equipment requirement; organic silicon with a branched structure is constructed through a sulfydryl-double bond click chemical reaction, and the reaction is rapid; the concave-convex effect organic film is manufactured by matching a branched structure with a sulfydryl-double bond structure and a long-chain alkyl structure, and the deepening proportion can reach 30%; the deepening agent does not contain fluorine, is green and environment-friendly, and overcomes the defects that the conventional deepening agent has poor hand feeling and needs subsequent hand feeling finishing.
Drawings
FIG. 1 shows H of the comb-shaped modified silicone oil of the present invention1-NMR spectrum.
FIG. 2 shows H of the comb-shaped modified silicone oil of the present invention1-partial enlargement of the NMR spectrum.
In the figure, the abscissa represents chemical shift, and the ordinate represents peak intensity.
Detailed Description
The embodiments described below with reference to the drawings are illustrative only and should not be construed as limiting the invention.
Example 1
(1) Preparing comb-shaped organic silicon: taking 500g of linear body, 12g of dodecyl methyl dimethoxy silane, 5g of mercaptopropyl methyl dimethoxy silane and 5g of N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane as raw materials, heating to 80 ℃, carrying out prepolymerization reaction for 0.5h under the action of 0.2g of sodium hydroxide, and carrying out vacuum decompression reaction for 2h to obtain the comb-shaped silicone oil.
(2) Preparation of branched silicone emulsion: adding 500g of comb-shaped organic silicon into a four-mouth flask with a thermometer, heating to 50 ℃, adding the comb-shaped organic silicon into the flask three times under the action of a triethanolamine catalyst, adding 4.07g of vinyl silicone oil with the molecular weight of 500g/mmol (if the vinyl is excessive, the comb-shaped organic silicon is added into the vinyl silicone oil) each time, and stirring for reacting for 30 minutes to obtain the organic silicone oil with the branched structure. Adding AEO-7 with the oil mass ratio of 30%, and adding deionized water under high-speed stirring for emulsification and dispersion to obtain the branched-structure organosilicon emulsion.
(3) The application process of the branched organosilicon emulsion comprises the following steps: and (3) carrying out heat setting on the working solution with the concentration of 20g/L by soaking and rolling-drying at 100 ℃ for-150 ℃ for 90 seconds.
Example 2
(1) Preparing comb-shaped organic silicon: taking 500g of linear body, 12g of dodecyl methyl dimethoxy silane, 5g of mercaptopropyl methyl dimethoxy silane and 5g of N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane as raw materials, heating to 80 ℃, carrying out prepolymerization reaction for 0.5h under the action of 0.2g of sodium hydroxide, and carrying out vacuum decompression reaction for 2h to obtain the comb-shaped silicone oil.
(2) Preparation of branched silicone emulsion: adding 500g of comb-shaped organic silicon into a four-mouth flask with a thermometer, heating to 50 ℃, adding the comb-shaped organic silicon into the flask three times under the action of a triethanolamine catalyst, adding 2g of vinyl silicone oil with the molecular weight of 500g/mmol (if the vinyl is excessive, the comb-shaped organic silicon is added into the vinyl silicone oil) each time, and stirring for reacting for 30 minutes to obtain the organic silicone oil with the branched structure. Adding AEO-7 with the oil mass ratio of 20%, and adding deionized water under high-speed stirring for emulsification and dispersion to obtain the branched-structure organosilicon emulsion.
(3) The application process of the branched organosilicon emulsion comprises the following steps: and (3) carrying out heat setting on the working solution with the concentration of 20g/L by soaking and rolling-drying at 100 ℃ for-150 ℃ for 90 seconds.
Example 3
(1) Preparing comb-shaped organic silicon: taking 500g of linear body, 12g of dodecyl methyl dimethoxy silane, 5g of mercaptopropyl methyl dimethoxy silane and 5g of N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane as raw materials, heating to 80 ℃, carrying out prepolymerization reaction for 0.5h under the action of 0.2g of sodium hydroxide, and carrying out vacuum decompression reaction for 2h to obtain the comb-shaped silicone oil.
(2) Preparation of branched silicone emulsion: adding 18g of vinyl silicone oil with the molecular weight of 500g/mmol into a four-neck flask with a thermometer, heating to 50 ℃, adding the vinyl silicone oil three times under the action of a triethanolamine catalyst, adding 167g of comb-shaped organic silicon (if the vinyl is excessive, the comb-shaped organic silicon is added into the vinyl silicone oil) each time, and stirring for reacting for 30 minutes to obtain the organic silicone oil with the branched structure. Adding AEO-7 with the oil mass ratio of 30%, and adding deionized water under high-speed stirring for emulsification and dispersion to obtain the branched-structure organosilicon emulsion.
(3) The application process of the branched organosilicon emulsion comprises the following steps: and (3) carrying out heat setting on the working solution with the concentration of 20g/L by soaking and rolling-drying at 100 ℃ for-150 ℃ for 90 seconds.
Example 4
(1) Preparing comb-shaped organic silicon: taking 500g of linear body, 12g of dodecyl methyl dimethoxy silane, 5g of mercaptopropyl methyl dimethoxy silane and 12g of N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane as raw materials, heating to 80 ℃, carrying out prepolymerization reaction for 1h under the action of 0.2g of sodium hydroxide, and carrying out vacuum pressure reduction reaction for 2h to obtain the comb-shaped silicone oil.
(2) Preparation of branched silicone emulsion: adding 500g of comb-shaped organic silicon into a four-mouth flask with a thermometer, heating to 50 ℃, adding the comb-shaped organic silicon into the flask three times under the action of a triethanolamine catalyst, adding 2g of vinyl silicone oil with the molecular weight of 500g/mmol (if the vinyl is excessive, the comb-shaped organic silicon is added into the vinyl silicone oil) each time, and stirring for reacting for 30 minutes to obtain the organic silicone oil with the branched structure. Adding AEO-7 with the oil mass ratio of 20%, and adding deionized water under high-speed stirring for emulsification and dispersion to obtain the branched-structure organosilicon emulsion.
(3) The application process of the branched organosilicon emulsion comprises the following steps: and (3) carrying out heat setting on the working solution with the concentration of 20g/L by soaking and rolling-drying at 100 ℃ for-150 ℃ for 90 seconds.
Example 5
(1) Preparing comb-shaped organic silicon: taking 500g of linear body, 12g of dodecyl methyl dimethoxy silane, 2g of mercaptopropyl methyl dimethoxy silane and 12g of N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane as raw materials, heating to 80 ℃, carrying out prepolymerization reaction for 1h under the action of 0.2g of sodium hydroxide, and carrying out vacuum pressure reduction reaction for 2h to obtain the comb-shaped silicone oil.
(2) Preparation of branched silicone emulsion: adding 500g of comb-shaped organic silicon into a four-mouth flask with a thermometer, heating to 50 ℃, adding the comb-shaped organic silicon into the four-mouth flask three times under the action of a triethanolamine catalyst, adding 1g of vinyl silicone oil with the molecular weight of 1000g/mmol (if the vinyl is excessive, the comb-shaped organic silicon is added into the vinyl silicone oil) each time, and stirring for reacting for 40 minutes to obtain the organic silicone oil with the branched structure. Adding AEO-7 with the oil mass ratio of 40%, and adding deionized water under high-speed stirring for emulsification and dispersion to obtain the branched-structure organosilicon emulsion.
(3) The application process of the branched organosilicon emulsion comprises the following steps: and (3) carrying out heat setting on the working solution with the concentration of 20g/L by soaking and rolling-drying at 100 ℃ for-150 ℃ for 90 seconds.
The total value of amino and sulfhydryl can be obtained by protonating amino and sulfhydryl of silicone oil in glacial acetic acid, and titrating the generated salt with hydrochloric acid standard solution under bromophenol blue indicator. And (3) the ammonia value + mercapto value is v C/m, wherein C is the equivalent concentration of the hydrochloric acid standard solution of 0.1, v is the volume of hydrochloric acid used for changing the titration solution from blue to yellow, and m is the mass of the required titration silicone oil.
In order to verify the structure of the comb-shaped silicone oil synthesized by the method, nuclear magnetic test is carried out.
Referring to FIGS. 1-2, it can be seen from H1-NMR spectrum 1-2 that strong-CH appears around 1.3ppm at δ2Methylene absorption peak, in the vicinity of 0.88ppm, -CH3Methyl Peak, Si-CH present at 0.1ppm3Silyl peak. The silicone oil has a long chain length of long chain alkyl groups and a high content of silicon methyl groupsmesosilyl-Si-CH3And methylene-CH2The intensity of the absorption peak is significantly greater than the other absorption peaks. The nuclear magnetism peak at the amplification delta of 1.5-4 ppm can be seen, and Si-CH can be seen at the amplification delta of 1.3ppm2Si-CH in the structures of mercapto-alkyl coupling agent and amino-alkyl coupling agent can be seen when the peak of silylene is 1.6ppm and the peak of delta is 1.7ppm2-CH2-, delta at 2.5ppm is-CH2NHCH2CH2NH2And CH2-SH。
In order to verify the darkening effect of the textile treated by the branched organosilicon darkening hand feeling finishing agent, the dE value and the darkening ratio are expressed.
The testing steps are as follows: 3 test specimens of 180 × 180mm (7 × 7in.) were conditioned for at least 4 hours at a temperature of 21 ± 1 ℃ and a relative humidity of 65 ± 2% in a standard environment before testing. In addition, each sample was required to contain all of the different gauge cd and md yarns in the face fabric. The sample was placed on a color difference meter, model VIS, manufactured by UltraScan, USA, and the dE value and the darkening ratio were read. The average value of three points measured by each piece of cloth is taken, and the average value of three pieces of cloth is taken for the same sample.
Example deepening scoring sheet
| Numbering | dE | Increasing the depth ratio |
| Example 1 | 2.53 | 32 |
| Example 2 | 2.24 | 29 |
| Example 3 | 2.26 | 29 |
| Example 4 | 2.17 | 28 |
| Example 5 | 2.31 | 30 |
The above description is only a preferred example of the present invention, and actually, the present invention can be realized by using the specific raw materials listed in the present invention, the upper and lower limits and interval values of each raw material, and the upper and lower limits and interval values of the process parameters (such as temperature, time, etc.), which are not listed herein.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents, and all such modifications as would be made without the inventive faculty are intended to be included within the scope of the invention.
Claims (1)
1. The application of the organic silicon emulsion darkening hand feeling finishing agent is characterized in that the structure of the organic silicon emulsion darkening hand feeling finishing agent is as follows:
the preparation method of the organic silicon emulsion darkening hand feeling finishing agent comprises the following steps: 1) preparing comb-shaped organic silicon: linear body, dodecyl methyl dimethoxy silane, mercaptopropyl methyl dimethoxy silane and N-beta-aminoethyl-gamma-aminopropyl methyl dimethoxy silane are adopted as raw materials, and are subjected to prepolymerization reaction for 0.5-4 h and vacuum decompression reaction for 1-10 h under the action of an alkaline catalyst to obtain the comb-shaped silicone oil with high affinity, soft hand feeling and good deepening effect;
2) preparation of branched silicone emulsion: adding comb-shaped organic silicon into a four-neck flask with a thermometer, heating to 50-70 ℃, adding vinyl silicone oil step by step under the action of a triethanolamine catalyst, and stirring for reaction for 30 minutes to 2 hours to obtain organic silicone oil with a branched structure; adding a surfactant, and adding deionized water under high-speed stirring for emulsification and dispersion to obtain a branched-structure organic silicon emulsion;
the organic silicon emulsion deepening hand feeling finishing agent is applied to fabric finishing, the concentration of a finishing liquid of the organic silicon emulsion deepening hand feeling finishing agent is not less than 20g/L, and the application process is as follows: 1) one step of dipping and one step of rolling; 2) drying at 100 ℃; 3) heat setting at 150-180 deg.c for 90 s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210142659.5A CN114541145A (en) | 2019-09-27 | 2019-09-27 | Application of organic silicon emulsion hand feeling deepening finishing agent |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910923252.4A CN110485166B (en) | 2019-09-27 | 2019-09-27 | Organic silicon emulsion hand feeling deepening finishing agent, preparation method and application |
| CN202210142659.5A CN114541145A (en) | 2019-09-27 | 2019-09-27 | Application of organic silicon emulsion hand feeling deepening finishing agent |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910923252.4A Division CN110485166B (en) | 2019-09-27 | 2019-09-27 | Organic silicon emulsion hand feeling deepening finishing agent, preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114541145A true CN114541145A (en) | 2022-05-27 |
Family
ID=68544190
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210142659.5A Pending CN114541145A (en) | 2019-09-27 | 2019-09-27 | Application of organic silicon emulsion hand feeling deepening finishing agent |
| CN201910923252.4A Active CN110485166B (en) | 2019-09-27 | 2019-09-27 | Organic silicon emulsion hand feeling deepening finishing agent, preparation method and application |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910923252.4A Active CN110485166B (en) | 2019-09-27 | 2019-09-27 | Organic silicon emulsion hand feeling deepening finishing agent, preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN114541145A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114541145A (en) * | 2019-09-27 | 2022-05-27 | 佛山市顺德区德美瓦克有机硅有限公司 | Application of organic silicon emulsion hand feeling deepening finishing agent |
| CN111116920B (en) * | 2019-12-26 | 2022-06-21 | 福建省晋江新德美化工有限公司 | Branched polyamino long-chain alkyl polysiloxane, waterproof soft organic silicon finishing agent and preparation method thereof |
| CN113914104B (en) * | 2021-10-26 | 2024-01-05 | 浙江金三发粘合衬有限公司 | Antibacterial crease-resistant cotton-flax fabric and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10140485A (en) * | 1996-11-08 | 1998-05-26 | Nippon Unicar Co Ltd | Color deepening agent comprising silicone-based block alternating copolymer |
| US6214961B1 (en) * | 1997-11-28 | 2001-04-10 | Shin-Etsu Chemical Co., Ltd. | Method of producing branched silicone oil |
| CN101446038A (en) * | 2008-12-31 | 2009-06-03 | 嘉兴银城精细化工有限公司 | Brightening agent for fabrics and production method thereof |
| CN105622944A (en) * | 2016-03-30 | 2016-06-01 | 科凯精细化工（上海）有限公司 | Quaternized organic silicone oil and preparation method thereof |
| CN108049186A (en) * | 2017-12-14 | 2018-05-18 | 佛山市顺德区德美瓦克有机硅有限公司 | Hydrophobic hand feel finishing agent of branched structure that a kind of acrylate is prepared with reactive silicone oil and preparation method thereof, application |
| CN108484933A (en) * | 2018-05-10 | 2018-09-04 | 浙江科峰新材料有限公司 | A kind of organic silicon emulsion and its production technology |
| CN110485166A (en) * | 2019-09-27 | 2019-11-22 | 佛山市顺德区德美瓦克有机硅有限公司 | A kind of organic silicon emulsion increases deep hand feel finishing agent and preparation method, application |
-
2019
- 2019-09-27 CN CN202210142659.5A patent/CN114541145A/en active Pending
- 2019-09-27 CN CN201910923252.4A patent/CN110485166B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10140485A (en) * | 1996-11-08 | 1998-05-26 | Nippon Unicar Co Ltd | Color deepening agent comprising silicone-based block alternating copolymer |
| US6214961B1 (en) * | 1997-11-28 | 2001-04-10 | Shin-Etsu Chemical Co., Ltd. | Method of producing branched silicone oil |
| CN101446038A (en) * | 2008-12-31 | 2009-06-03 | 嘉兴银城精细化工有限公司 | Brightening agent for fabrics and production method thereof |
| CN105622944A (en) * | 2016-03-30 | 2016-06-01 | 科凯精细化工（上海）有限公司 | Quaternized organic silicone oil and preparation method thereof |
| CN108049186A (en) * | 2017-12-14 | 2018-05-18 | 佛山市顺德区德美瓦克有机硅有限公司 | Hydrophobic hand feel finishing agent of branched structure that a kind of acrylate is prepared with reactive silicone oil and preparation method thereof, application |
| CN108484933A (en) * | 2018-05-10 | 2018-09-04 | 浙江科峰新材料有限公司 | A kind of organic silicon emulsion and its production technology |
| CN110485166A (en) * | 2019-09-27 | 2019-11-22 | 佛山市顺德区德美瓦克有机硅有限公司 | A kind of organic silicon emulsion increases deep hand feel finishing agent and preparation method, application |
| CN110485166B (en) * | 2019-09-27 | 2022-04-08 | 佛山市顺德区德美瓦克有机硅有限公司 | Organic silicon emulsion hand feeling deepening finishing agent, preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110485166B (en) | 2022-04-08 |
| CN110485166A (en) | 2019-11-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110485166B (en) | Organic silicon emulsion hand feeling deepening finishing agent, preparation method and application | |
| CN104892832B (en) | A kind of preparation method of micro-cross-linked polymethyl acyloxyethyl trimethyl ammonium chloride modification color fixing agent | |
| CN104711852B (en) | Finishing method of cotton-hydrophobic fabric based on BTCA-TEOS-OA combined treatment | |
| CN111996815B (en) | Preparation and dyeing of boron/silicon-containing hybrid functional protein fiber | |
| CN112127157B (en) | Polyamino acid graft modified water-repellent fabric and preparation method thereof | |
| CN112962311B (en) | POSS (polyhedral oligomeric silsesquioxane) -based sulfhydryl-alkene click chemistry method for preparing super-hydrophobic textile | |
| CN109056320B (en) | Flame-retardant hydrophobic finishing method based on cotton fabric | |
| CN110983801A (en) | Preparation method of waterproof moisture-permeable cotton fabric | |
| CN103015186B (en) | Carbon black treating agent for synthetic leather and preparation method of carbon black treating agent | |
| CN112853754A (en) | Water-repellent anti-ultraviolet polyester and preparation method thereof | |
| CN112194638B (en) | Aniline anhydride, preparation method thereof and polyamino acid graft chain | |
| CN112900089B (en) | Waterproof fiber knitted fabric and preparation method thereof | |
| CN114197209A (en) | Skin-feel fabric | |
| CN114059363A (en) | Preparation process of polyester sanded wax-like printed cloth | |
| CN109295769B (en) | Preparation method of silk with ultraviolet radiation prevention function | |
| CN111647128B (en) | Preparation method of formaldehyde-free textile color fixing agent | |
| CN112981989B (en) | Printing and dyeing additive and method for dyeing real silk/viscose composite fabric | |
| CN110818875A (en) | Organic silicon modified polyurethane, application thereof and preparation method of coated fabric of organic silicon modified polyurethane | |
| CN110565369A (en) | Treatment method for improving fastness to soaping and fading of yarn dyed fabric and yarn dyed fabric | |
| CN111979794B (en) | Functional modification method for improving dyeing effect of natural dye alkaline bath for fabric | |
| CN114163644B (en) | Softening deepening agent and preparation method thereof | |
| CN108532329A (en) | A kind of one-bath process softening agent and preparation method thereof | |
| CN117510859A (en) | Deepening agent for silk fabric low-temperature dyeing and preparation and application methods thereof | |
| CN113047044B (en) | Anti-wrinkle and anti-fatigue school uniform and preparation process thereof | |
| CN113493311B (en) | Transparent silicon dioxide antireflection film coating process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |