CN102964601B - Formula and synthesis process of novel block hydrophilic silicone oil - Google Patents
Formula and synthesis process of novel block hydrophilic silicone oil Download PDFInfo
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- CN102964601B CN102964601B CN201210478813.2A CN201210478813A CN102964601B CN 102964601 B CN102964601 B CN 102964601B CN 201210478813 A CN201210478813 A CN 201210478813A CN 102964601 B CN102964601 B CN 102964601B
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- silicone oil
- hydrophilic silicone
- block hydrophilic
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 11
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920000570 polyether Polymers 0.000 claims abstract description 16
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 15
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229960000583 acetic acid Drugs 0.000 claims abstract description 9
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 150000004985 diamines Chemical class 0.000 claims description 14
- 125000003700 epoxy group Chemical group 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000001117 sulphuric acid Substances 0.000 claims description 8
- 235000011149 sulphuric acid Nutrition 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000003921 oil Substances 0.000 abstract description 10
- 229910052710 silicon Inorganic materials 0.000 abstract description 7
- 239000010703 silicon Substances 0.000 abstract description 7
- 150000002825 nitriles Chemical class 0.000 abstract description 4
- 239000004744 fabric Substances 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 3
- 239000004677 Nylon Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 229920001778 nylon Polymers 0.000 abstract description 2
- 229920000728 polyester Polymers 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 2
- 210000002268 wool Anatomy 0.000 abstract 2
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 abstract 1
- 229920000742 Cotton Polymers 0.000 abstract 1
- 239000004593 Epoxy Substances 0.000 abstract 1
- 125000003277 amino group Chemical group 0.000 abstract 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract 1
- 230000008961 swelling Effects 0.000 abstract 1
- -1 amido silicon Chemical compound 0.000 description 6
- DUFKCOQISQKSAV-UHFFFAOYSA-N Polypropylene glycol (m w 1,200-3,000) Chemical class CC(O)COC(C)CO DUFKCOQISQKSAV-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- 229920004933 Terylene® Polymers 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229920013822 aminosilicone Polymers 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 235000010855 food raising agent Nutrition 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
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- Silicon Polymers (AREA)
Abstract
The invention discloses block hydrophilic silicon oil, in particular discloses formula and synthesis process of novel block hydrophilic silicone oil. The invention aims to provide a formula and synthesis process of a novel block hydrophilic silicone oil, which are low in manufacturing cost, simple in process and environment-friendly. According to the formula, the novel block hydrophilic silicone oil comprises aliphatic polyethenoxyamine isopropanol, epoxy-terminated silicon oil, 20% sulfuric acid solution, dipropylene glycol, isooctanol polyethenoxy ether and glacial acetic acid. The production process is simple, the prepared block hydrophilic silicone oil manufactured is linear multiblock modified organic siloxane, and epoxy, polyether, amine group and the like are intercalated in the molecule main chain of the block hydrophilic silicone oil, and the prepared block hydrophilic silicone oil is particularly used for softness after-finishing of various loose wool, yarns, textiles and fabrics of polyester, nylon, nitrile, blended wool and nitrile, purified cotton and the like; in addition, the prepared environment-friendly swelling agent does not contain chemical components such as formaldehyde, NP/APEO (alkylphenol ethoxylates) and heavy metal, thereby being very environment-friendly.
Description
Technical field
The present invention relates to a kind of block hydrophilic silicone oil, especially a kind of formula of novel block hydrophilic silicone oil and synthesis technique.
Background technology
In the hand feel finishing agent of textiles, all need to use amido silicon oil in the market.Amido silicon oil is that grow up the eighties in last century a kind of is mainly used in softness, the modified silicon oil that fluffy, smooth hand arranges, but amido silicon oil can not directly be used, must add after emulsifying agent is emulsified into dairy industry and could use, due to amido silicon oil easy problem such as breakdown of emulsion, floating oil, generation silicone oil spot in the process of using.In addition, in amido silicon oil, contain the chemical compositions such as formaldehyde, NP/APEO and heavy metal, there is higher contaminative.
In recent years, the block silicone oil of substituted-amino silicone oil product progressively came into vogue on market, but due to synthetic operation more complicated, and raw material dependence on import causes that block silicone oil quality on market is unstable, cost is higher.
Summary of the invention
The object of the invention is to provide in order to solve the deficiency of above-mentioned technology that a kind of low cost of manufacture, technique are simple, formula and the synthesis technique of a kind of novel block hydrophilic silicone oil of environmental protection.
In order to achieve the above object, the formula of a kind of novel block hydrophilic silicone oil that the present invention is designed, it comprises 35-45 part aliphatic poly ether diamine, 300-340 part Virahol, 360-400 part epoxy group(ing) end-blocking silicone oil, the sulphuric acid soln that 4-6 part concentration is 20%, 400-450 part dipropylene glycol, 150-170 part isomery polyoxyethylenated alcohol and 1-3 part Glacial acetic acid, above umber is calculated by weight.
As preferably, the aliphatic poly ether diamine that the aliphatic poly ether diamine that described aliphatic poly ether diamine is 900 by molecular weight and molecular weight are 2000 forms, and the two quality equates.
Production technique: the first step, by 35-45 part aliphatic poly ether diamine, 300-340 part Virahol, 360-400 part epoxy group(ing) end-blocking silicone oil is put in reactor together, is heated to 80 ℃, insulation reaction 8 hours; Second step, adds the sulphuric acid soln that 4-6 part concentration is 20%, balanced reaction 30 minutes; The 3rd step, adds 400-450 part dipropylene glycol, balanced reaction 30 minutes, and negative pressure vacuumizes, and is warming up to 100 ℃, and vacuum tightness is evacuated to the highest, takes out most volatile matter Virahol, and balanced reaction 30 minutes is cooled to 50 ℃; The 4th step, adds 150-170 part isomery polyoxyethylenated alcohol and 1-3 part Glacial acetic acid, stirs, and is cooled to 35 ℃, discharging.
Formula and the synthesis technique of the resulting a kind of novel block hydrophilic silicone oil of the present invention, production technique is simple, the block hydrophilic silicone oil manufacturing is that the polynary block modified organosilicon of a kind of linearity is supported alkane, on molecular backbone chain, embed epoxy group(ing), polyethers and amino etc., be exclusively used in terylene, nylon, nitrile, the blending of hair nitrile, blend polyester and after the softness of various loose hairs, yarn, fabric and the fabric such as textile, arrange; In addition, the environmental protection leavening agent that the present invention makes is not containing the chemical compositions such as formaldehyde, NP/APEO and heavy metal, very environmental protection.
Accompanying drawing explanation
Nothing.
Embodiment
Embodiment 1:
Formula and the synthesis technique of a kind of novel block hydrophilic silicone oil that the present embodiment is described, the first step, by 45 parts of aliphatic poly ether diamines, 340 parts of Virahols, 400 parts of epoxy group(ing) end-blocking silicone oil are put in reactor together, are heated to 80 ℃, insulation reaction 8 hours; Second step, adds the sulphuric acid soln that 6 parts of concentration are 20%, balanced reaction 30 minutes; The 3rd step, adds 450 parts of dipropylene glycols, balanced reaction 30 minutes, and negative pressure vacuumizes, and is warming up to 100 ℃, and vacuum tightness is evacuated to the highest, takes out most volatile matter Virahol, and balanced reaction 30 minutes is cooled to 50 ℃; The 4th step, adds 170 parts of isomery polyoxyethylenated alcohol and 3 parts of Glacial acetic acid, stirs, and is cooled to 35 ℃, discharging.
Embodiment 2:
Formula and the synthesis technique of a kind of novel block hydrophilic silicone oil that the present embodiment is described, the first step, by 35 parts of aliphatic poly ether diamines, 300 parts of Virahols, 360 parts of epoxy group(ing) end-blocking silicone oil are put in reactor together, are heated to 80 ℃, insulation reaction 8 hours; Second step, adds the sulphuric acid soln that 4 parts of concentration are 20%, balanced reaction 30 minutes; The 3rd step, adds 400 parts of dipropylene glycols, balanced reaction 30 minutes, and negative pressure vacuumizes, and is warming up to 100 ℃, and vacuum tightness is evacuated to the highest, takes out most volatile matter Virahol, and balanced reaction 30 minutes is cooled to 50 ℃; The 4th step, adds 150 parts of isomery polyoxyethylenated alcohol and 1 part of Glacial acetic acid, stirs, and is cooled to 35 ℃, discharging.
Embodiment 3:
Formula and the synthesis technique of a kind of novel block hydrophilic silicone oil that the present embodiment is described, the first step, by 40 parts of aliphatic poly ether diamines, 320 parts of Virahols, 380 parts of epoxy group(ing) end-blocking silicone oil are put in reactor together, are heated to 80 ℃, insulation reaction 8 hours; Second step, adds the sulphuric acid soln that 5 parts of concentration are 20%, balanced reaction 30 minutes; The 3rd step, adds 420 parts of dipropylene glycols, balanced reaction 30 minutes, and negative pressure vacuumizes, and is warming up to 100 ℃, and vacuum tightness is evacuated to the highest, takes out most volatile matter Virahol, and balanced reaction 30 minutes is cooled to 50 ℃; The 4th step, adds 160 parts of isomery polyoxyethylenated alcohol and 2 parts of Glacial acetic acid, stirs, and is cooled to 35 ℃, discharging.
Claims (3)
1. a novel block hydrophilic silicone oil, it is characterized in that: its raw material comprises 35-45 part aliphatic poly ether diamine, 300-340 part Virahol, 360-400 part epoxy group(ing) end-blocking silicone oil, the sulphuric acid soln that 4-6 part concentration is 20%, 400-450 part dipropylene glycol, 150-170 part isomery polyoxyethylenated alcohol and 1-3 part Glacial acetic acid, above umber is calculated by weight; Its production method: the first step, by 35-45 part aliphatic poly ether diamine, 300-340 part Virahol, 360-400 part epoxy group(ing) end-blocking silicone oil is put in reactor together, is heated to 80 ℃, insulation reaction 8 hours; Second step, adds the sulphuric acid soln that 4-6 part concentration is 20%, balanced reaction 30 minutes; The 3rd step, adds 400-450 part dipropylene glycol, balanced reaction 30 minutes, and negative pressure vacuumizes, and is warming up to 100 ℃, and vacuum tightness is evacuated to the highest, takes out most volatile matter Virahol, and balanced reaction 30 minutes is cooled to 50 ℃; The 4th step, adds 150-170 part isomery polyoxyethylenated alcohol and 1-3 part Glacial acetic acid, stirs, and is cooled to 35 ℃, discharging.
2. a kind of novel block hydrophilic silicone oil according to claim 1, is characterized in that: the aliphatic poly ether diamine that the aliphatic poly ether diamine that described aliphatic poly ether diamine is 900 by molecular weight and molecular weight are 2000 forms, and the two quality equates.
3. a synthesis technique for novel block hydrophilic silicone oil, is characterized in that: the first step, by 35-45 part aliphatic poly ether diamine, 300-340 part Virahol, 360-400 part epoxy group(ing) end-blocking silicone oil is put in reactor together, is heated to 80 ℃, insulation reaction 8 hours; Second step, adds the sulphuric acid soln that 4-6 part concentration is 20%, balanced reaction 30 minutes; The 3rd step, adds 400-450 part dipropylene glycol, balanced reaction 30 minutes, and negative pressure vacuumizes, and is warming up to 100 ℃, and vacuum tightness is evacuated to the highest, takes out most volatile matter Virahol, and balanced reaction 30 minutes is cooled to 50 ℃; The 4th step, adds 150-170 part isomery polyoxyethylenated alcohol and 1-3 part Glacial acetic acid, stirs, and is cooled to 35 ℃, discharging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210478813.2A CN102964601B (en) | 2012-11-21 | 2012-11-21 | Formula and synthesis process of novel block hydrophilic silicone oil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210478813.2A CN102964601B (en) | 2012-11-21 | 2012-11-21 | Formula and synthesis process of novel block hydrophilic silicone oil |
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| Publication Number | Publication Date |
|---|---|
| CN102964601A CN102964601A (en) | 2013-03-13 |
| CN102964601B true CN102964601B (en) | 2014-11-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210478813.2A Active CN102964601B (en) | 2012-11-21 | 2012-11-21 | Formula and synthesis process of novel block hydrophilic silicone oil |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5807956A (en) * | 1996-03-04 | 1998-09-15 | Osi Specialties, Inc. | Silicone aminopolyalkyleneoxide block copolymers |
-
2012
- 2012-11-21 CN CN201210478813.2A patent/CN102964601B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5807956A (en) * | 1996-03-04 | 1998-09-15 | Osi Specialties, Inc. | Silicone aminopolyalkyleneoxide block copolymers |
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| CN102964601A (en) | 2013-03-13 |
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Address after: Hong Yuan Lu Tongxiang Puyuan sweater City Industrial Park of Jiaxing City, Zhejiang province 314500 Patentee after: Zhejiang Quping Textile New Materials Co., Ltd. Address before: Hong Yuan Lu Tongxiang Puyuan sweater City Industrial Park of Jiaxing City, Zhejiang province 314500 Patentee before: Jiaxing Queping Textile Chemical Industry Co., Ltd. |