CN106543445A - Super soft and smooth silicone oil of a kind of SRS D9 types and preparation method thereof - Google Patents
Super soft and smooth silicone oil of a kind of SRS D9 types and preparation method thereof Download PDFInfo
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- CN106543445A CN106543445A CN201610959294.XA CN201610959294A CN106543445A CN 106543445 A CN106543445 A CN 106543445A CN 201610959294 A CN201610959294 A CN 201610959294A CN 106543445 A CN106543445 A CN 106543445A
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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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- 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
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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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
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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Abstract
The invention belongs to textile dyeing and finishing technical field, and in particular to super soft and smooth silicone oil of a kind of SRS D9 types and preparation method thereof.The super soft and smooth silicone oil of the present invention, the raw material comprising following weight portion：40～60 parts of dimethicone mixture, 1～5 part of tetramethyldihydrogendisiloxane, 1～5 part of the concentrated sulfuric acid, 2～8 parts of sodium acid carbonate, 1～5 part of allyl glycidyl ether, chloroplatinic acid：0.1～0.6 part, 10～20 parts of isopropanol, 15～30 parts of polyetheramine, 5～15 parts of aliphatic alcohol polyethenoxy base ether.The super soft and smooth silicone oil of the present invention not only can improve weaving with giving excellent flexibility, smoothness, bulkiness, fullness after block modified sillicon oil treatment fabric, the advantages of being organized the hydrophily of fabric, acid and alkali-resistance, resistance to hard water simultaneously can also be improved, field and wide application prospect is had a wide range of applications.
Description
Technical field
The invention belongs to textile dyeing and finishing technical field, and in particular to a kind of super soft and smooth silicone oil of SRS-D9 types and its preparation side
Method.
Background technology
In order to improve the wearability of textile, improving product added value improves the class of product, textile is carried out soft
Soft arrangement is one of critically important approach.It is soft, fluffy that amido silicon oil is that the one kind for growing up the eighties in last century is mainly used in
The modified silicon oil that pine, smooth hand are arranged, with chemical characteristics such as stronger polarity, reactivity, adsorptivities, improves fabric hand
Sense, be allowed to it is soft, smooth, well-pressed, with the function such as elastic, crease-resistant, imitate so as to imparting amido silicon oil and arranging in fabric feeling
Geneogenous advantage on fruit, and it is friendly to human body, thus it is well received.But amido silicon oil can be just made after must adding emulsifying agent
With, developing through technology for many years, the aspect such as the selection of amino silicone oil emulsifying agent, optimization of emulsifying process has obtained thoroughly changing
Become, but still easy breakdown of emulsion during can not inherently solving amido silicon oil use, floating oil, roll banding, glue cylinder, be also easy to produce silicone oil spot etc.
Problem, meanwhile, the introducing of the highly active amino of side chain result in the easy discoloration of fabric, xanthochromia, the fabric after process and can not return something for repairs
A series of problem.Simultaneously amido silicon oil also makes scrim present certain hydrophobicity, reduce fabric hygroscopicity and
Sense comfortable and easy to wear, in recent years, the block silicone oil of substituted-amino silicone oil product is progressively commercially developed,
In order to overcome the shortcoming of traditional amido silicon oil, people to carry out using various new technologies, new method by technological innovation
Technological improvement, the property modifying functional group of excellent and the linear polymer of silicone backbone one, this is that organic silicone oil is soft
One new stage of soft dose of development, and the developing direction that textile dyeing and finishing process is inevitable.
The content of the invention
Goal of the invention：The purpose of the present invention is provided a kind of linear multiple copolymerized block and changes for the deficiencies in the prior art
Property silicone softening agent, give the excellent pliability of fabric, smooth degree, a kind of super soft and smooth silicone oil of SRS-D9 types of fluffy degree and
Its preparation method.
Technical scheme：In order to realize the purpose of the present invention, the present invention is implemented by below scheme：A kind of SRS-D9 types are super soft
Sliding silicone oil, each group distribution ratio calculated by following raw materials by weight portion are made：
40～60 parts of dimethicone mixture
1～5 part of tetramethyldihydrogendisiloxane
1～5 part of the concentrated sulfuric acid
2～8 parts of sodium acid carbonate
1～5 part of allyl glycidyl ether
Chloroplatinic acid：0.1～0.6 part
10～20 parts of isopropanol
15～30 parts of polyetheramine
5～15 parts of aliphatic alcohol polyethenoxy base ether
Further optimize, a kind of super soft and smooth silicone oil of SRS-D9 types of the present invention, each group distribution ratio counted by weight is：
50 parts of dimethicone mixture
3 parts of tetramethyldihydrogendisiloxane
1.5 parts of the concentrated sulfuric acid
2.5 parts of sodium acid carbonate
3.5 parts of allyl glycidyl ether
Chloroplatinic acid：0.4 part
16 parts of isopropanol
25 parts of polyetheramine
10 parts of aliphatic alcohol polyethenoxy base ether
A kind of preparation method of the super soft and smooth silicone oil of SRS-D9 types of the present invention, comprises the following steps：
(1) first by dimethicone mixture, tetramethyldihydrogendisiloxane, be added to it is closed with stirring warding off
In porcelain reaction pot, stirring is opened, the concentrated sulfuric acid is slowly added dropwise, and is heated to 40～60 DEG C, 4～8h of synthetic reaction；
(2) then in reaction pot sodium acid carbonate is added to be neutralized reaction, adjustment pH value is to 7, and maintains the temperature at 50
～55 DEG C, uniform stirring 30min；Then filtered using filter, filtrate is obtained Jing after separation of solid and liquid.
(3), after the completion of filtering, filtrate is transferred in the closed enamel reaction pot with stirring, allyl glycidol is added
Ether, isopropanol, chloroplatinic acid are opened stirring, are heated to 90～130 DEG C, 4～8h of chain extending reaction；Polyetheramine is subsequently added into, is adjusted
Whole temperature to 100～130 DEG C, 4～8h of addition reaction.
(4) after completion of the reaction, cool down material and be cooled to 40 DEG C, addition aliphatic alcohol polyethenoxy base ether, uniform stirring 1h, i.e.,
A kind of super soft and smooth silicone oil of SRS-D9 types is obtained.
Sulfuric acid solution of the described concentrated sulfuric acid for mass fraction 98.5%.
Beneficial effects of the present invention
The super soft and smooth silicone oil of a kind of SRS-D9 types that the present invention is provided, the siloxane unit of preparation of adopting new technology can reach
2000 and more than, far above the 1000 or so of current synthesis technique.The silicone oil not only can improve weaving and use block modified silicone oil
Excellent flexibility, smoothness, bulkiness, fullness are given after finish fabric, while the parent for being organized fabric can also be improved
It is aqueous.
Specific embodiment
Below by instantiation, the present invention is described in detail.
Embodiment 1：
A kind of super soft and smooth silicone oil of SRS-D9 types of the present invention, its preparation method are comprised the following steps：
(1) first by 500kg dimethicone mixtures, 30kg tetramethyldihydrogendisiloxanes, be added to it is closed
In 1000L enamel reaction pot with stirring, stirring is opened, the concentrated sulfuric acid solution that 15kg mass fractions are 98.5% is slowly added dropwise,
And 55 DEG C are heated to, synthetic reaction 6h；
(2) then in reaction pot 25kg sodium acid carbonates are added to be neutralized reaction, adjustment pH value is to 7, and keeping temperature
At 52 DEG C, uniform stirring 30min；Then filtered using filter, obtained filtrate material.
(3) filtrate material is transferred in the closed 2000L enamel reaction pots with stirring, adds 35kg allyl glycidyls sweet
Oily ether, 160kg isopropanols, 4kg chloroplatinic acids are opened stirring, are heated to 110 DEG C, chain extending reaction 5h；It is subsequently added into 250kg
Polyetheramine, adjustment temperature to 120 DEG C, addition reaction 6h.
(4) after completion of the reaction, cool down material and be cooled to 40 DEG C, add 100kg aliphatic alcohol polyethenoxy base ethers, uniform stirring
1h, after sampling detection is qualified, blowing packaging is obtained a kind of super soft and smooth silicone oil of SRS-D9 types.
Embodiment 2：
A kind of super soft and smooth silicone oil of SRS-D9 types of the present invention, its preparation method are comprised the following steps：
(1) first by 550kg dimethicone mixtures, 35kg tetramethyldihydrogendisiloxanes, be added to it is closed
In 1000L enamel reaction pot with stirring, stirring is opened, the concentrated sulfuric acid solution that 16kg mass fractions are 98.5% is slowly added dropwise,
And 58 DEG C are heated to, synthetic reaction 7h；
(2) then in reaction pot 28kg sodium acid carbonates are added to be neutralized reaction, adjustment pH value is to 7, and keeping temperature
At 53 DEG C, uniform stirring 30min；Then filtered using filter, obtained filtrate material.
(3) filtrate material is transferred in the closed 2000L enamel reaction pots with stirring, adds 40kg allyl glycidyls sweet
Oily ether, 180kg isopropanols, 5kg chloroplatinic acids are opened stirring, are heated to 120 DEG C, chain extending reaction 6h；It is subsequently added into 280kg
Polyetheramine, adjustment temperature to 125 DEG C, addition reaction 6.5h.
(4) after completion of the reaction, cool down material and be cooled to 40 DEG C, add 120kg aliphatic alcohol polyethenoxy base ethers, uniform stirring
1h, after sampling detection is qualified, blowing packaging is obtained a kind of super soft and smooth silicone oil of SRS-D9 types.
Embodiment 3：
A kind of super soft and smooth silicone oil of SRS-D9 types of the present invention, its preparation method are comprised the following steps：
(1) first by 450kg dimethicone mixtures, 25kg tetramethyldihydrogendisiloxanes, be added to it is closed
In 1000L enamel reaction pot with stirring, stirring is opened, the concentrated sulfuric acid solution that 12kg mass fractions are 98.5% is slowly added dropwise,
And 50 DEG C are heated to, synthetic reaction 5.5h；
(2) then in reaction pot 21kg sodium acid carbonates are added to be neutralized reaction, adjustment pH value is to 7, and keeping temperature
At 51 DEG C, uniform stirring 30min；Then filtered using filter, obtained filtrate material.
(3) filtrate material is transferred in the closed 2000L enamel reaction pots with stirring, adds 28kg allyl glycidyls sweet
Oily ether, 140kg isopropanols, 3kg chloroplatinic acids are opened stirring, are heated to 105 DEG C, chain extending reaction 5.5h；It is subsequently added into
220kg polyetheramines, adjustment temperature to 115 DEG C, addition reaction 5.5h.
(4) after completion of the reaction, cool down material and be cooled to 40 DEG C, add 85kg aliphatic alcohol polyethenoxy base ethers, uniform stirring
1h, after sampling detection is qualified, blowing packaging is obtained a kind of super soft and smooth silicone oil of SRS-D9 types.
The super soft and smooth silicone oil of a kind of SRS-D9 types obtained in embodiment 1--3 is carried out into performance test, Jing is super, and soft and smooth silicone oil is processed
Fabric test result afterwards is as shown in table 1:
Table 1：The property indices of product in embodiment 1～3
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Slippery (level) | 5 | 4.5 | 4.5 |
| Pliability (level) | 5 | 5 | 5 |
| Richness (level) | 5 | 5 | 5 |
| Hydrophily | ＜ 1s | ＜ 1s | ＜ 1s |
| Acid resistance (PH=2) | It is stable | It is stable | It is stable |
| Alkali resistance (PH=10) | It is stable | It is stable | It is stable |
| Resistance to hard water (600ppm) | It is stable | It is stable | It is stable |
Above a kind of super soft and smooth silicone oil of SRS-D9 types provided by the present invention is described in detail.It is used herein
Specific case is set forth to the principle and embodiment of the present invention, and the explanation of above example is only intended to help and understands this
The core concept of invention.It should be pointed out that for those skilled in the art, without departing from the principle of the invention
Under the premise of, some improvement and modification can also be carried out to the present invention.These improve and modification should also be as falling into right of the present invention will
In the protection domain asked.
Claims (4)
1. super soft and smooth silicone oil of a kind of SRS-D9 types and preparation method thereof, it is characterised in that its each component in terms of parts by weight is matched somebody with somebody
Than for：40～60 parts of dimethicone mixture, 1～5 part of tetramethyldihydrogendisiloxane, 1～5 part of the concentrated sulfuric acid, carbonic acid
2～8 parts of hydrogen sodium, 1～5 part of allyl glycidyl ether, chloroplatinic acid：0.1～0.6 part, 10～20 parts of isopropanol, polyetheramine 15～
30 parts, 5～15 parts of aliphatic alcohol polyethenoxy base ether.
2. super soft and smooth silicone oil of a kind of SRS-D9 types according to claim 1 and preparation method thereof, it is characterised in that further
Optimize, each group distribution ratio counted by weight is：50 parts of dimethicone mixture, tetramethyldihydrogendisiloxane 3
Part, 1.5 parts of the concentrated sulfuric acid, 2.5 parts of sodium acid carbonate, 3.5 parts of allyl glycidyl ether, chloroplatinic acid：0.4 part, it is 16 parts of isopropanol, poly-
25 parts of ether amines, 10 parts of aliphatic alcohol polyethenoxy base ether.
3. super soft and smooth silicone oil of a kind of SRS-D9 types according to claim 1 and preparation method thereof, it is characterised in that described
Sulfuric acid solution of the concentrated sulfuric acid for mass fraction 98.5%.
4. super soft and smooth silicone oil of a kind of SRS-D9 types according to claim 1 and preparation method thereof, it is characterised in that by following
Concrete steps are made：
(1) first by dimethicone mixture, tetramethyldihydrogendisiloxane, be added to it is closed with stirring enamel it is anti-
In answering pot, stirring is opened, the concentrated sulfuric acid is slowly added dropwise, and is heated to 40～60 DEG C, 4～8h of synthetic reaction；
(2) then in reaction pot sodium acid carbonate is added to be neutralized reaction, adjustment pH value is to 7, and maintains the temperature at 50～55
DEG C, uniform stirring 30min；Then filtered using filter, filtrate is obtained Jing after separation of solid and liquid.
(3), after the completion of filtering, filtrate is transferred in the closed enamel reaction pot with stirring, allyl glycidyl ether is added,
Isopropanol, chloroplatinic acid are opened stirring, are heated to 90～130 DEG C, 4～8h of chain extending reaction；Polyetheramine is subsequently added into, is adjusted
Temperature to 100～130 DEG C, 4～8h of addition reaction.
(4) after completion of the reaction, cool down material and be cooled to 40 DEG C, add aliphatic alcohol polyethenoxy base ether, uniform stirring 1h to be obtained
A kind of super soft and smooth silicone oil of SRS-D9 types.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610959294.XA CN106543445A (en) | 2016-11-03 | 2016-11-03 | Super soft and smooth silicone oil of a kind of SRS D9 types and preparation method thereof |
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| CN201610959294.XA CN106543445A (en) | 2016-11-03 | 2016-11-03 | Super soft and smooth silicone oil of a kind of SRS D9 types and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617863A (en) * | 2012-03-30 | 2012-08-01 | 广东工业大学 | Preparation method of hydrophilic block polyether aminosilicone |
| CN104031269A (en) * | 2014-05-20 | 2014-09-10 | 江阴市诺科科技有限公司 | Hydrophilic block polyether amino silicone oil with amino branched chain, and preparation method and application thereof |
| CN104707365A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Preparation method of amino polyether organic silicon compounded antifoaming agent |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
-
2016
- 2016-11-03 CN CN201610959294.XA patent/CN106543445A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617863A (en) * | 2012-03-30 | 2012-08-01 | 广东工业大学 | Preparation method of hydrophilic block polyether aminosilicone |
| CN104707365A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Preparation method of amino polyether organic silicon compounded antifoaming agent |
| CN104031269A (en) * | 2014-05-20 | 2014-09-10 | 江阴市诺科科技有限公司 | Hydrophilic block polyether amino silicone oil with amino branched chain, and preparation method and application thereof |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
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Application publication date: 20170329 |