CN103643527A - Preparation method of ring-shaped silicone softener - Google Patents
Preparation method of ring-shaped silicone softener Download PDFInfo
- Publication number
- CN103643527A CN103643527A CN201310688109.4A CN201310688109A CN103643527A CN 103643527 A CN103643527 A CN 103643527A CN 201310688109 A CN201310688109 A CN 201310688109A CN 103643527 A CN103643527 A CN 103643527A
- Authority
- CN
- China
- Prior art keywords
- grams
- preparation
- temperature
- vacuum
- ring
- 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.)
- Granted
Links
Landscapes
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of a ring-shaped silicone softener, including a synthetic method of epoxy ring-shaped silicon oil and a synthetic method of a ring-shaped silicone softener. According to the technical solution provided by the invention, the preparation method comprises the steps of introducing an organic silicon ring body of a ball-ring structure on a main chain of organic silicon to form a ring-shaped molecular internal space, thus increasing a macromolecular internal space distance and a rotating space of a silica chain segment so as to improve bulkiness, rebound resilience and flexibility of a textile processed by the softener, overcoming problems and shortcomings in the prior art that a processed textile is in lack of bulkiness, rebound resilience and flexibility. The textile processed by the ring-shaped silicone softener can be improved in bulkiness, rebound resilience and flexibility.
Description
Technical field
The present invention relates to a kind of preparation method of fabric of organosilicon softener, specifically refer to for fabric being carried out to the preparation method of a kind of ring type structure silicone softening agent of resilience, pliability, bulkiness arrangement.
Background technology
Fabric of organosilicon softener claims again silicone softening agent, the silicone softening agent that prior art arranges for textiles soft feel, mainly contain the modified silicon oil of amino-modified silicone oil, polynary block silicone oil, emulsion polymerisation, these silicone based softeners are the main octamethylcy-clotetrasiloxane (D that adopts in synthetic process
4) or the organosilicon polymer of dimethyl siloxane mixed methylcyclosiloxane (DMC) linear structure of ring-opening polymerization under the effect of alkalescence or acidic catalyst, the main body of structure is linear silica segment (Si-O), silicon oxygen bond its flexibility in all chemical constitutions is best, thereby the silicone softening agent of having given linear structure has excellent softness, level and smooth effect.The silicone softening agent of linear structure is processed on textile fabric can form fine and close organosilicone film uniformly, but due to tightr between molecular structure, there is no space in enough molecules, cause the resilience of silicone softening agent finish fabric of linear structure poor, fabric after wherethrough reason is too soft, lacks bulkiness, resilience and pliability; Therefore, prior art exists processed fabric to lack bulkiness, resilience and flexible problems and shortcomings.
Summary of the invention
The problems and shortcomings that exist for above-mentioned prior art, the present invention adopts the organosilicon ring body of introducing ball structure on organosilyl main chain, form space in ring-like molecule, utilize the revolution space that increases intramolecular space length and silica segment, improve the bulkiness of the textiles of wherethrough reason, resilience and flexible technical scheme, a kind of preparation method of ring type structure silicone softening agent is provided, be intended to by preparing ring type structure silicone softening agent, for fabric is processed, make processed fabric reach raising bulkiness, resilience and flexible object.
The object of the present invention is achieved like this: a kind of preparation method of ring type structure silicone softening agent, comprise synthesizing epoxy ring body silicone oil method and synthetic ring type structure organosilicon flexible agent method, wherein:
Described synthesizing epoxy ring body silicone oil method, comprises A formula and A preparation method,
Described A fills a prescription,
Organic silicon monomer: 1,2,2,3,3,4,5,5,6,6-decamethyl-Isosorbide-5-Nitrae-dihydro ring, six siloxanes, 416 grams;
Modifier: allyl glycidyl ether, 285 grams;
Catalyst: the platinum acid chloride solution of mass percent concentration 1%, 1.4 grams;
Described A preparation method is, synthetic,
Modifier in described A formula and catalyst are dropped in there-necked flask, then slowly stir and heat up, stir speed (S.S.) is 100 revs/min, when temperature is raised to 70 ℃ ± 2 ℃, slowly splash into the organic silicon monomer in described A formula, in the process dripping, exothermic reaction can occur, adopt cold water water-bath cooling, drop rate is controlled with the temperature rise of exothermic reaction, drip process temperature and be controlled at 70 ℃～82 ℃, drip and finish, keep 80 ℃ ± 5 ℃ insulations of temperature to continue stirring reaction 5～6 hours, reaction is finished; Afterwards, vacuum is pulled out modifier excessive in reactant liquor: vacuum is 0.099MPa, and it is 120 ℃ that vacuum is pulled out temperature, and the modifier amount of pulling out is 58.4 grams; Afterwards, cool to room temperature, obtain 644 grams of epoxy ring body silicone oil;
Described synthetic ring type structure organosilicon flexible agent method, comprises B formula and B preparation method,
Described B fills a prescription,
The epoxy ring body silicone oil being obtained by described A preparation method, 644 grams;
Curing agent: α, ω-bis-aminopropyl dimethyl silicone polymer, 396 grams; (be commonly called as: end amido silicon oil)
Solvent: isopropyl alcohol, 500 grams;
Described B preparation method is, synthetic
Epoxy ring body silicone oil, curing agent and solvent in described B formula are dropped in there-necked flask, stir and heat up, stir speed (S.S.) is 100 revs/min, and temperature is controlled at 80 ℃ ± 5 ℃, insulation reaction 10 hours, and reaction is finished; Afterwards, vacuum is pulled out solvent excessive in reactant liquor, and vacuum is 0.099MPa, and it is 80 ℃ that vacuum is pulled out temperature, and the solvent amount of pulling out is 400 grams, afterwards, cools to room temperature, obtains 1140 grams of ring type structure silicone softening agents.
Above-mentioned, the present invention adopts the organosilicon ring body of introducing ball structure on organosilyl main chain, form space in ring-like molecule, utilize the revolution space that increases intramolecular space length and silica segment, improve the bulkiness of the textiles of wherethrough reason, resilience and flexible technical scheme, having overcome prior art exists processed fabric to lack bulkiness, resilience and flexible problems and shortcomings, the preparation method of a kind of ring type structure silicone softening agent providing, by preparing ring type structure silicone softening agent for fabric is processed, make processed fabric reach raising bulkiness, resilience and flexible object.
Embodiment explanation
By specific embodiment, the preparation method of a kind of ring type structure silicone softening agent of the present invention is described in further detail below, those skilled in the art can make ring type structure silicone softening agent with reference to formula and the preparation method of embodiment, but should not be construed as any limitation of the invention.
The specific embodiment
Embodiment
The name of an article: ring type structure silicone softening agent
Preparation
Preparation condition, equipment
Ambient pressure a: atmospheric pressure;
Environment temperature: room temperature;
Preparation equipment and supporting: there-necked flask, supporting water-bath cooler, electric heater, agitator and vacuum source;
The first step, synthesizing epoxy ring body silicone oil, comprise A formula and A preparation method,
A fills a prescription,
Organic silicon monomer: 1,2,2,3,3,4,5,5,6,6-decamethyl-Isosorbide-5-Nitrae-dihydro ring, six siloxanes, 416 grams;
Modifier: allyl glycidyl ether, 285 grams;
Catalyst: the platinum acid chloride solution of mass percent concentration 1%, 1.4 grams;
A preparation method is, synthetic,
Modifier in described A formula and catalyst are dropped in there-necked flask, then slowly stir and heat up, stir speed (S.S.) is 100 revs/min, when temperature is raised to 70 ℃ ± 2 ℃, slowly splash into the organic silicon monomer in described A formula, in the process dripping, exothermic reaction can occur, adopt cold water water-bath cooling, drop rate is controlled with the temperature rise of exothermic reaction, drip process temperature and be controlled at 70 ℃～82 ℃, drip and finish, keep 80 ℃ ± 5 ℃ insulations of temperature to continue stirring reaction 5～6 hours, reaction is finished; Afterwards, vacuum is pulled out modifier excessive in reactant liquor: vacuum is 0.099MPa, and it is 120 ℃ that vacuum is pulled out temperature, and the modifier amount of pulling out is 58.4 grams; Afterwards, cool to room temperature, obtain 644 grams of epoxy ring body silicone oil;
Second step, synthetic ring type structure silicone softening agent, comprise B formula and B preparation method,
B fills a prescription,
The epoxy ring body silicone oil being obtained by described A preparation method, 644 grams;
Curing agent: α, ω-bis-aminopropyl dimethyl silicone polymer, 396 grams; (be commonly called as: end amido silicon oil)
Solvent: isopropyl alcohol, 500 grams;
Described B preparation method is, synthetic
Epoxy ring body silicone oil, curing agent and solvent in described B formula are dropped in there-necked flask, stir and heat up, stir speed (S.S.) is 100 revs/min, and temperature is controlled at 80 ℃ ± 5 ℃, insulation reaction 10 hours, and reaction is finished; Afterwards, vacuum is pulled out solvent excessive in reactant liquor, and vacuum is 0.099MPa, and it is 80 ℃ that vacuum is pulled out temperature, and the solvent amount of pulling out is 400 grams, afterwards, cools to room temperature, obtains 1140 grams of ring type structure silicone softening agents.
Claims (1)
1. a preparation method for ring type structure silicone softening agent, comprises synthesizing epoxy ring body silicone oil method and synthetic ring type structure organosilicon flexible agent method, it is characterized in that:
Described synthesizing epoxy ring body silicone oil method, comprises A formula and A preparation method,
Described A fills a prescription,
Organic silicon monomer: 1,2,2,3,3,4,5,5,6,6-decamethyl-Isosorbide-5-Nitrae-dihydro ring, six siloxanes, 416 grams;
Modifier: allyl glycidyl ether, 285 grams;
Catalyst: the platinum acid chloride solution of mass percent concentration 1%, 1.4 grams;
Described A preparation method is, synthetic,
Modifier in described A formula and catalyst are dropped in there-necked flask, then slowly stir and heat up, stir speed (S.S.) is 100 revs/min, when temperature is raised to 70 ℃ ± 2 ℃, slowly splash into the organic silicon monomer in described A formula, in the process dripping, exothermic reaction can occur, adopt cold water water-bath cooling, drop rate is controlled with the temperature rise of exothermic reaction, drip process temperature and be controlled at 70 ℃～82 ℃, drip and finish, keep 80 ℃ ± 5 ℃ insulations of temperature to continue stirring reaction 5～6 hours, reaction is finished; Afterwards, vacuum is pulled out modifier excessive in reactant liquor: vacuum is 0.099MPa, and it is 120 ℃ that vacuum is pulled out temperature, and the modifier amount of pulling out is 58.4 grams; Afterwards, cool to room temperature, obtain 644 grams of epoxy ring body silicone oil;
Described synthetic ring type structure organosilicon flexible agent method, comprises B formula and B preparation method,
Described B fills a prescription,
The epoxy ring body silicone oil being obtained by described A preparation method, 644 grams;
Curing agent: α, ω-bis-aminopropyl dimethyl silicone polymer, 396 grams; (be commonly called as: end amido silicon oil)
Solvent: isopropyl alcohol, 500 grams;
Described B preparation method is, synthetic
Epoxy ring body silicone oil, curing agent and solvent in described B formula are dropped in there-necked flask, stir and heat up, stir speed (S.S.) is 100 revs/min, and temperature is controlled at 80 ℃ ± 5 ℃, insulation reaction 10 hours, and reaction is finished; Afterwards, vacuum is pulled out solvent excessive in reactant liquor, and vacuum is 0.099MPa, and it is 80 ℃ that vacuum is pulled out temperature, and the solvent amount of pulling out is 400 grams, afterwards, cools to room temperature, obtains 1140 grams of ring type structure silicone softening agents.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310688109.4A CN103643527B (en) | 2013-12-07 | 2013-12-07 | A kind of preparation method of ring type structure silicone softening agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310688109.4A CN103643527B (en) | 2013-12-07 | 2013-12-07 | A kind of preparation method of ring type structure silicone softening agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103643527A true CN103643527A (en) | 2014-03-19 |
| CN103643527B CN103643527B (en) | 2015-09-16 |
Family
ID=50248805
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310688109.4A Active CN103643527B (en) | 2013-12-07 | 2013-12-07 | A kind of preparation method of ring type structure silicone softening agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103643527B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951422A (en) * | 2016-05-13 | 2016-09-21 | 无为县荣华鬃刷制品有限公司 | Solution capable of improving flexibility of bristles |
| CN112482031A (en) * | 2020-11-27 | 2021-03-12 | 苏州联胜化学有限公司 | Fluffy elastic silicone oil for terylene and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634036A (en) * | 2012-05-14 | 2012-08-15 | 上海德周化工有限公司 | Novel linear amino and polyester modified organosilicon compound for textiles |
| CN103113590A (en) * | 2013-01-16 | 2013-05-22 | 杭州美高华颐化工有限公司 | Quaternary ammonium base organopolysiloxane high-molecular compound and preparation method and application thereof |
| KR101284152B1 (en) * | 2012-06-20 | 2013-07-17 | 윤강훈 | Silicon copolymer, its manufacturing method and fabric softner using the same |
-
2013
- 2013-12-07 CN CN201310688109.4A patent/CN103643527B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634036A (en) * | 2012-05-14 | 2012-08-15 | 上海德周化工有限公司 | Novel linear amino and polyester modified organosilicon compound for textiles |
| KR101284152B1 (en) * | 2012-06-20 | 2013-07-17 | 윤강훈 | Silicon copolymer, its manufacturing method and fabric softner using the same |
| CN103113590A (en) * | 2013-01-16 | 2013-05-22 | 杭州美高华颐化工有限公司 | Quaternary ammonium base organopolysiloxane high-molecular compound and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951422A (en) * | 2016-05-13 | 2016-09-21 | 无为县荣华鬃刷制品有限公司 | Solution capable of improving flexibility of bristles |
| CN112482031A (en) * | 2020-11-27 | 2021-03-12 | 苏州联胜化学有限公司 | Fluffy elastic silicone oil for terylene and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103643527B (en) | 2015-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4029629A (en) | Solvent resistant room temperature vulcanizable silicone rubber composition | |
| CN106317409A (en) | Preparing method of polyorganosiloxane microsphere | |
| CN105297427B (en) | A kind of compound for improving amino-modified silicone oil based carbon fiber finish heat resistance and its preparation and application | |
| CN103601889B (en) | A kind of polyol ester modified silicon oil, preparation method and carbon fiber oil preparation | |
| CN109384929A (en) | A kind of organosilicon cross-linking agent and preparation method thereof containing polyhedral oligomeric silsesquioxane structure | |
| CN103819680B (en) | A kind of preparation method of methoxyl group end-blocking amino-modified silicone oil | |
| CN109880585A (en) | A kind of liquid silastic and preparation method thereof of pair of selective bonding of plastic basis material | |
| CN107556471A (en) | A kind of non-isocyanate organic silicon polyurethane block copolymer and its synthetic method | |
| CN105037768A (en) | Method for preparing organic silicon modified chitosan membrane | |
| CN107400241A (en) | A kind of preparation method of containing hydrogen silicone oil | |
| CN103643527B (en) | A kind of preparation method of ring type structure silicone softening agent | |
| CN104109244B (en) | A kind of long chain fluorine-containing alkyl-silicone oil and synthetic method thereof | |
| CN104356390A (en) | Organosiloxane containing benzocyclobutene group as well as preparation method and application thereof | |
| CN110156997A (en) | It is a kind of can moisture solidification organic silicon block copolymer and preparation method thereof | |
| CN104140535B (en) | A kind of MQ silicones containing phenyl and preparation method thereof | |
| CN108997582A (en) | A kind of preparation method of the single-ended polysiloxane fluid containing active hydrogen | |
| KR20180071263A (en) | Process for producing hydrosilyl group-containing organosilicon resin | |
| CN104108216B (en) | A kind of method adopting radial copolymer modification antireflective polyester film | |
| CN108864433A (en) | thermoplastic silicone material and preparation method | |
| CN105601934B (en) | Modified double-end amino dimethyl silicone polymer of ammonia hydrocarbyl side chain and preparation method thereof | |
| CN103881387A (en) | Addition-type antistatic silicone rubber | |
| CN113004524A (en) | Epoxy-organic silicon resin and preparation method and application thereof | |
| CN115710826B (en) | Giant tow carbon fiber precursor oiling agent and preparation method thereof | |
| CN105254897B (en) | Methylphenyl-piperazinyl modified polyorganosiloxane | |
| CN105418670B (en) | Poly- (acetenyl dimethyl silica) silsesquioxane of cage modle eight and its synthetic method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: 315600, No. 10, Jinlong Road, C District, Xinxing Development Zone, Ninghai County, Zhejiang, Ningbo Patentee after: Ningbo run Wo hi tech materials Polytron Technologies Inc Address before: 315600, No. 10, Jinlong Road, C District, Xinxing Industrial Park, Ninghai County, Zhejiang, Ningbo Patentee before: Ningbo Runhe Chemical Industry Co., Ltd. |
|
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: No. 168, Jinhai Middle Road, Binhai New Area, South Ningbo, Ninghai County, Ningbo City, Zhejiang Province Patentee after: NINGBO RUNHE HIGH-TECH MATERIAL Co.,Ltd. Address before: 315600, No. 10, Jinlong Road, C District, Xinxing Development Zone, Ninghai County, Zhejiang, Ningbo Patentee before: NINGBO RUNHE HIGH-TECH MATERIAL Co.,Ltd. |