CN109734933A - Organic silicon emulsion and preparation method thereof for the processing of synthetic leather artificial leather surface slip - Google Patents
Organic silicon emulsion and preparation method thereof for the processing of synthetic leather artificial leather surface slip Download PDFInfo
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- CN109734933A CN109734933A CN201811622975.2A CN201811622975A CN109734933A CN 109734933 A CN109734933 A CN 109734933A CN 201811622975 A CN201811622975 A CN 201811622975A CN 109734933 A CN109734933 A CN 109734933A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- 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
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
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- 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
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M15/6433—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing carboxylic groups
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/10—Block- or graft-copolymers containing polysiloxane sequences
- C08J2383/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Textile Engineering (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
The invention discloses a kind of organic silicon emulsions and preparation method thereof for the processing of synthetic leather artificial leather surface slip, and the organic silicon emulsion includes each component of following mass ratio: silicone oil of carboxyl crude oil: emulsifier: water 30-35:2-8:50-65；Wherein, the silicone oil of carboxyl crude oil is formed by dimethyl siloxane mixed methylcyclosiloxane, closure agent, carboxy-silane coupling agent and catalyst by polycondensation reaction.The waterborne organic silicon lotion applied to synthetic leather artificial leather surface that the present invention is prepared, good with artificial leather surface adhesion force, feel conservation degree is high after rubbing line；And preparation process is simple, emulsion particle diameter obtained is thin, and floating oil, stability is not good in printing process.
Description
Technical field
The present invention relates to organic silicon emulsions and preparation method thereof, sliding for synthetic leather artificial leather surface more particularly to one kind
The organic silicon emulsion and preparation method thereof of refreshing processing.
Background technique
Mostly use hydroxy silicon oil, methyl-silicone oil and amino silicon oil emulsion as the surface treating agent of smooth processing greatly at present,
But its major defect is:
(1) hydroxyl, methyl-silicone oil emulsion partial size are big, and printing is poor；
(2) existing hydroxy silicon oil, methyl-silicone oil and amido silicon oil are in printing process due to the extruding meeting of blade and roller
Cause to be demulsified, final finished product leather surface is made oil mark occur；
(3) to the poor adhesive force of leather, feel conservation degree is weak for hydroxy silicon oil, methyl-silicone oil emulsion.
Therefore, develop that a kind of preparation process is simple, printing is good, the good organic silicon emulsion of adhesive force is artificial to synthetic leather
Leather surface treatment has great importance.
Summary of the invention
Of the existing technology in order to solve the problems, such as, the present invention provides one kind at synthetic leather artificial leather surface slip
Organic silicon emulsion of reason and preparation method thereof, to improve the printing and adhesive force and stability of surface treating agent.
To achieve the above object, the technical solution adopted by the present invention is that a kind of handled for synthetic leather artificial leather surface slip
Organic silicon emulsion:
Each component including following mass ratio:
Silicone oil of carboxyl crude oil: emulsifier: water 30-35:2-8:50-65；
Wherein, the silicone oil of carboxyl crude oil is grouped as by each group of following parts by weight:
In one embodiment of the invention, the structural formula of the carboxy-silane coupling agent is Si-PEG-COOH.
In one embodiment of the invention, the specific structure of the carboxy-silane coupling agent is (OMe)3Si(CH2)2NHCONH
(CH2)2(EO) mCOOH or (OEt)3Si(CH2)2NHCONH(CH2)2(EO) mCOOH, wherein m >=3.
In one embodiment of the invention, the closure agent is hexamethyldisiloxane.
In one embodiment of the invention, the catalyst is acid cation exchange resin.
In one embodiment of the invention, the emulsifier is fatty alcohol polyoxyethylene ether.
A kind of preparation method of organic silicon emulsion, which comprises the following steps:
A, dimethyl siloxane mixed methylcyclosiloxane, closure agent, carboxy-silane coupling agent and acid cation exchange resin are existed
Polycondensation is mixed in container, polycondensation reaction obtains polycondensation product；
B, the obtained polycondensation product of step a is evaporated under reduced pressure, terminates distillation after constant mass, cooling obtains carboxyl silicon
Oily crude oil；
C, silicone oil of carboxyl, emulsifier and water that step b is obtained are added to the container, stirring and emulsifying, obtain transparent carboxyl
Silicone oil emulsion.
In one embodiment of the invention, the stirring in step c is the mechanical stirring carried out at normal temperature.
In one embodiment of the invention, the reaction temperature of polycondensation is 100-200 DEG C.
The technical program has the advantages that
The present invention has synthesized a kind of silicone oil of carboxyl lotion, first by carboxy-silane coupling agent, dimethyl siloxane mixed methylcyclosiloxane
And closure agent and catalyst carry out polycondensation reaction at a certain temperature, obtain the silicone oil of carboxyl that side chain is carboxyl, then by the carboxylic
Base silicone oil obtains silicone oil of carboxyl lotion of the invention by emulsifier.The present invention solves hydroxy silicon oil and methyl-silicone oil is logical
Instability problem caused by a large amount of emulsifier compoundings is crossed, obtained silicone oil of carboxyl good emulsion stability, adhesive force is strong,
And partial size is small, printing is good, and oil mark is not generated in printing process.
Specific embodiment
The present invention will be further described below with reference to examples.
Embodiment 1
The preparation of silicone oil of carboxyl crude oil:
By octamethylcy-clotetrasiloxane, hexamethyldisiloxane, carboxy-silane coupling agent and acid cation exchange resin
Polycondensation is mixed in a reservoir, and mass ratio is respectively 4000:15:250:1, and the reaction temperature of polycondensation is 120 DEG C, the reaction time 4
Hour.Silicone oil of carboxyl crude oil required for being obtained after being evaporated under reduced pressure.In the present embodiment, used carboxy-silane coupling agent
General formula is Si-PEG-COOH, specially (OMe) 3Si (CH2) 2NHCONH (CH2) 2 (EO) mCOOH, wherein m >=3.
The preparation of silicone oil of carboxyl lotion:
Silicone oil of carboxyl crude oil, fatty alcohol polyoxyethylene ether and the water of preparation are added to the container, mass ratio is respectively 32:
4:64 carries out mechanical agitation emulsification, mixing speed 1000r/min under room temperature, and mixing time is 1 hour, obtains transparent and stable
Silicone oil of carboxyl lotion, remember lotion 1.
Using test:
The silicone oil of carboxyl lotion is carried out following performance test: (1) centrifugal stability is tested, and test condition is revolving speed
3000r/min, time 30min；(2) printing is tested, and test condition is 300 mesh roller printings, time 30min, observation
Whether the edge of a knife has grease
(3) feel assessment test, test condition are to print the lotion, 80 DEG C of dry rubs 30 of temperature in 300 mesh of synthetic leather surface
Minute.Test result: lotion 1 is centrifuged not stratified, and prints the edge of a knife without oil mark, the glossy sense of leather surface good hand feeling is strong.
Embodiment 2
The preparation of silicone oil of carboxyl crude oil:
By octamethylcy-clotetrasiloxane, hexamethyldisiloxane, carboxy-silane coupling agent and acid cation exchange resin
Polycondensation is mixed in a reservoir, and mass ratio is respectively 3500:20:250:1, and the reaction temperature of polycondensation is 120 DEG C, the reaction time 4
Hour.Silicone oil of carboxyl crude oil required for being obtained after being evaporated under reduced pressure.In the present embodiment, used carboxy-silane coupling agent
General formula is Si-PEG-COOH, specially (OMe) 3Si (CH2) 2NHCONH (CH2) 2 (EO) mCOOH, wherein m >=3.
The preparation of silicone oil of carboxyl lotion:
Silicone oil of carboxyl crude oil, fatty alcohol polyoxyethylene ether and the water of preparation are added to the container, mass ratio is respectively 33:
3:64 carries out mechanical agitation emulsification, mixing speed 1000r/min under room temperature, and mixing time is 1 hour, obtains transparent and stable
Silicone oil of carboxyl lotion, remember lotion 2.
Using test:
The silicone oil of carboxyl lotion is carried out following performance test: (1) centrifugal stability is tested, and test condition is revolving speed
3000r/min, time 30min；(2) printing is tested, and test condition is 300 mesh roller printings, time 30min, observation
Whether the edge of a knife has grease
(3) feel assessment test, test condition are to print the lotion, 80 DEG C of dry rubs 30 of temperature in 300 mesh of synthetic leather surface
Minute.Test result: lotion 2 be centrifuged it is not stratified, and print the edge of a knife without oil mark, but due to closure agent excessively cause synthesis carboxyl
Silicone molecule amount is lower, therefore leather surface feel is poorer than lotion 1, and glossy sense is insufficient.
Embodiment 3
The preparation of silicone oil of carboxyl crude oil:
Octamethylcy-clotetrasiloxane, hexamethyl siloxane, carboxy-silane coupling agent and acid cation exchange resin are existed
Polycondensation is mixed in container, mass ratio is respectively 4500:10:150:1, and the reaction temperature of polycondensation is 120 DEG C, and the reaction time 4 is small
When.Silicone oil of carboxyl crude oil required for being obtained after being evaporated under reduced pressure.In the present embodiment, used carboxy-silane coupling agent leads to
Formula is Si-PEG-COOH, specially (OEt) 3Si (CH2) 2NHCONH (CH2) 2 (EO) mCOOH, wherein m >=3.
The preparation of silicone oil of carboxyl lotion:
Silicone oil of carboxyl crude oil, fatty alcohol polyoxyethylene ether and the water of preparation are added to the container, mass ratio is respectively 35:
7:58 carries out mechanical agitation emulsification, mixing speed 1000r/min under room temperature, and mixing time is 1 hour, obtains translucent steady
Fixed silicone oil of carboxyl lotion remembers lotion 3.
Using test:
The silicone oil of carboxyl lotion is carried out following performance test: (1) centrifugal stability is tested, and test condition is revolving speed
3000r/min, time 30min；(2) printing is tested, and test condition is 300 mesh roller printings, time 30min, observation
Whether the edge of a knife has grease
(3) feel assessment test, test condition are to print the lotion, 80 DEG C of dry rubs 30 of temperature in 300 mesh of synthetic leather surface
Minute.Test result: the centrifugation of lotion 3 has a small amount of layering, and centrifugal stability is poor, carboxy-silane when this may be synthesized with silicone oil of carboxyl
It is few to be coupled agent content, the silicone oil is caused to be not easy to emulsify.Meanwhile printing the edge of a knife has a small amount of oil mark to be precipitated, also some are greasy for feel.
Comparative example
Methyl-silicone oil emulsion preparation:
It is that 5000cps, fatty alcohol polyoxyethylene ether and water are added to the container by commercially available methyl-silicone oil viscosity, mass ratio
Respectively 35:7:58 carries out mechanical agitation emulsification, mixing speed 1000r/min under room temperature, and mixing time is 1 hour, obtains
Milky methyl-silicone oil emulsion remembers lotion 4.
Using test:
Methyl-silicone oil emulsion is carried out following performance test: (1) centrifugal stability is tested, and test condition is revolving speed 3000r/
Min, time 30min；(2) printing is tested, and test condition is 300 mesh roller printings, and time 30min, observing the edge of a knife is
It is no to have grease
(3) feel assessment test, test condition are to print the lotion, 80 DEG C of dry rubs 30 of temperature in 300 mesh of synthetic leather surface
Minute.Test result: the centrifugation layering of lotion 4 is serious, and centrifugal stability is poor, and the edge of a knife has a large amount of oil marks to be precipitated after five minutes for printing, uses
For lotion 4 in synthetic leather surface printing, feel is very greasy, uncomfortable.
The selection carboxy-silane coupling agent of novelty of the invention prepares silicone oil of carboxyl using mass polymerization, shows with current
Some silicone oil of carboxyl preparation methods are compared, and have simple production process, the few advantage of side reaction.And contain polyethers in silicone oil of carboxyl
Key improves hydrophily, keeps the silicone oil emulsion of emulsification more stable；Emulsion particle diameter is thin, not floating oil in printing process.Meanwhile with
Artificial leather surface adhesion force is good, and feel conservation degree is high after rubbing line.Also find out with comparative example through the foregoing embodiment, the present invention is made
Standby stability of organic silicone emulsion has large increase, therefore can have stronger applicability in industrial application.
Above-mentioned specific embodiment is used only to illustrate the present invention, rather than is to limit the invention, in the present invention
Objective and scope of protection of the claims in, to any replacement and change not made the creative labor for making of the present invention,
Fall within the scope of protection of the patent of the present invention.
Claims (10)
1. a kind of organic silicon emulsion for the processing of synthetic leather artificial leather surface slip, which is characterized in that including following mass ratio
Each component:
Silicone oil of carboxyl crude oil: emulsifier: water 30-35:2-8:50-65；
Wherein, the silicone oil of carboxyl crude oil is grouped as by each group of following parts by weight:
2. the organic silicon emulsion according to claim 1 for the processing of synthetic leather artificial leather surface slip, which is characterized in that
The general formula of the carboxy-silane coupling agent is Si-PEG-COOH.
3. the organic silicon emulsion according to claim 2 for the processing of synthetic leather artificial leather surface slip, which is characterized in that
The specific structure of the carboxy-silane coupling agent is (OMe)3Si(CH2)2NHCONH(CH2)2(EO) mCOOH or (OEt)3Si
(CH2)2NHCONH(CH2)2(EO) mCOOH, wherein m >=3.
4. the organic silicon emulsion according to claim 1 for the processing of synthetic leather artificial leather surface slip, which is characterized in that
The closure agent is hexamethyldisiloxane.
5. the organic silicon emulsion according to claim 1 for the processing of synthetic leather artificial leather surface slip, which is characterized in that
The catalyst is acid cation exchange resin.
6. the organic silicon emulsion according to claim 1 for the processing of synthetic leather artificial leather surface slip, which is characterized in that
The emulsifier is fatty alcohol polyoxyethylene ether.
7. a kind of preparation method according to any organic silicon emulsion of right 1-5, which comprises the following steps:
A, by dimethyl siloxane mixed methylcyclosiloxane, closure agent, carboxy-silane coupling agent and acid cation exchange resin in container
Middle mixing polycondensation, polycondensation reaction obtain polycondensation product；
B, the obtained polycondensation product of step a is evaporated under reduced pressure, terminates distillation after constant mass, cooling obtains silicone oil of carboxyl original
Oil；
C, silicone oil of carboxyl, emulsifier and water that step b is obtained are added to the container, stirring and emulsifying, obtain transparent silicone oil of carboxyl
Lotion.
8. the preparation method of organic silicon emulsion according to claim 5, which is characterized in that the stirring in step c is normal
The lower mechanical stirring carried out of temperature.
9. the preparation method of organic silicon emulsion according to claim 5, which is characterized in that the reaction temperature of polycondensation is 100-
200℃。
10. the preparation method of organic silicon emulsion according to claim 5, which is characterized in that the time of polycondensation reaction is
3.5-4.5h。
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| CN202111210998.4A CN113788959B (en) | 2018-12-28 | 2018-12-28 | Preparation method of organic silicon emulsion |
| CN201811622975.2A CN109734933B (en) | 2018-12-28 | 2018-12-28 | Organic silicon emulsion for surface smooth treatment of synthetic leather and preparation method thereof |
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| CN110552207A (en) * | 2019-10-10 | 2019-12-10 | 嘉兴冰火新材料科技有限公司 | Wear-resistant and scratch-resistant material for leather and preparation method thereof |
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| CN110552207A (en) * | 2019-10-10 | 2019-12-10 | 嘉兴冰火新材料科技有限公司 | Wear-resistant and scratch-resistant material for leather and preparation method thereof |
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| CN113788959B (en) | 2023-11-17 |
| CN113788959A (en) | 2021-12-14 |
| CN109734933B (en) | 2021-09-24 |
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