CN107286348A - A kind of preparation method of antistatic additive polyether modified silicon oil processed - Google Patents
A kind of preparation method of antistatic additive polyether modified silicon oil processed Download PDFInfo
- Publication number
- CN107286348A CN107286348A CN201710641129.4A CN201710641129A CN107286348A CN 107286348 A CN107286348 A CN 107286348A CN 201710641129 A CN201710641129 A CN 201710641129A CN 107286348 A CN107286348 A CN 107286348A
- Authority
- CN
- China
- Prior art keywords
- parts
- modified silicon
- silicon oil
- polyether modified
- preparation
- 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
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
- C08G77/32—Post-polymerisation treatment
- C08G77/34—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Analytical Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides a kind of preparation method of antistatic additive polyether modified silicon oil processed, it is characterised in that preparation method comprises the following steps：By weight, by 100 parts of polyethers, 80 180 parts of containing hydrogen silicone oil, 15 parts of chloroplatinic acids, 10 30 parts of isopropanols, react 2 6h at a temperature of nitrogen environment, 80 110 DEG C, product is through filtering, separation, obtains polyether modified silicon oil crude product, polyether modified silicon oil crude product is passed through in the chromatographic column equipped with high-efficiency adsorbent, flow velocity 0.5BV, that is, obtain high-purity polyether modified silicon oil product.
Description
Technical field
The present invention relates to a kind of preparation method of polyether modified silicon oil, especially a kind of polyether-modified silicon of antistatic additive processed
The preparation method of oil.
Background technology
Polyether modified silicon oil is a kind of organosilicon nonionic surfactant of unique properties.It has good lubrication
Property, lower surface tension, more preferable flexible nature and antistatic property, good levelability, can improve resin well
Intermolecular stress, overcomes the shortcoming of these resins in itself, obtains new performance, it has preferable breaking, it is adaptable to certain
The water-oil separating of a little specific occasions, this product, can be miscible with water with arbitrary proportion compared with dimethyl silicone polymer, also with polarity
Organic solvent such as alcohol, DMF, ether, ester etc. dissolve each other, and are partially or completely mixed with the non-polar solven such as toluene, alkane.It is easy to use,
Application field is extensive.
CN105504289A discloses a kind of preparation method of polyether modified silicon oil, including：Urged in porous ceramics Supported Pt Nanoparticles
In the presence of agent, the polyethers of terminal alkene group and containing hydrogen silicone oil are subjected to hydrosilylation in a solvent, filtered, filter is collected
Liquid；The filtrate is removed into solvent, polyether modified silicon oil is obtained.
CN105435490A discloses a kind of polyether silicone oil paraffin defoamer, including following components in percentage by weight：20
~40% polyethers, 20~35% dimethicone, 10~25% water, 10~15% carbon black and 10~15% stone
Wax.Meanwhile, the invention also discloses the preparation method of above-mentioned defoamer.
Polyether modified silicon oil can be used as defoamer, levelling agent applied to industrial circle, while being also widely used in day
Normal sphere of life, such as fabric finishing agent, cosmetic field etc., existing polyether modified silicon oil production technology is mostly using simple
Filter, the method progress product purification such as charcoal absorption, the impurity such as the easy remainder catalyst of product, raw material for being produced causes
It is unsuitable for applying to daily use chemicals, the daily life field such as textile finishing, and influences properties of product, while may cause product face
Colour cast is yellow, therefore, and researching and developing a kind of high-efficiency adsorbent easily used is extremely necessary.
The content of the invention
The purpose of the present invention is：A kind of preparation method of antistatic additive polyether modified silicon oil processed is provided, it is characterised in that
Step includes：
1. the preparation of adsorbent
By weight, by 100 parts of sepharose hydrophobic interaction medium, 0.1-1 parts of 3- oxo aza ring butyl- 1- carboxylic acid tert-butyl esters,
(R)-(+) 0.1-1 parts of -3- amido tetrahydrofurans tosilate, (1- (2- (trimethylsilyl) ethoxymethyl)) -1H-
0.5-2 parts of imidazoles -2- methylamine hydrochlorides, are added in 200-500 parts of DMFs, anti-at a temperature of 60-100 DEG C
6-15h is answered, product is dried through separation, obtains adsorbent product of the present invention.
2. the preparation of polyether modified silicon oil
By weight, by 100 parts of polyethers, 80-180 parts of containing hydrogen silicone oil, 1-5 parts of chloroplatinic acids, 10-30 parts of isopropanols, in nitrogen
Environment, 2-6h is reacted at a temperature of 80-110 DEG C, and product obtains polyether modified silicon oil crude product through filtering, separation, will be polyether-modified
Silicone oil crude product is passed through in the chromatographic column of the adsorbent produced equipped with step 1, and flow velocity 0.5BV obtains high-purity polyether-modified
Silicone oil product.
Described sepharose hydrophobic interaction medium is commercially available prod, as Xi'an indigo plant dawn scientific and technological new material Co., Ltd produces
Product；3- oxo aza ring butyl- 1- carboxylic acid tert-butyl esters are commercially available prod, the production of the rich chemical Science and Technology Ltd.'s production of such as Shanghai speed
Product；(R)-(+) -3- amido tetrahydrofurans tosilate is commercially available prod, such as the product of Shanghai Si Yu chemical companies production；
(1- (2- (trimethylsilyl) ethoxymethyl)) -1H- imidazoles -2- methylamine hydrochlorides are commercially available prod, the proper wind in such as Nanjing and doctor
The product of medicine Science and Technology Ltd. production.Polyethers, containing hydrogen silicone oil is commercially available prod.
The product of the present invention has the advantages that：
The adsorbent product that the present invention is produced, has the characteristics of specific surface area is big, in the identical time, compared to activated carbon
Deng conventional adsorbent, the amount of adsorbing contaminant is bigger, and is more applicable for adsorbing the remaining catalysis contained in polyether modified silicon oil
Agent, a small amount of Residual reactants so that the polyether modified silicon oil product purity produced is high, functional.
Embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
1. the preparation of adsorbent
In 1000L high-speed stirred kettles, the tertiary fourth of sepharose hydrophobic interaction medium 100Kg, 3- oxo aza ring butyl- 1- carboxylic acids is added
Ester 0.5Kg, (R)-(+) -3- amido tetrahydrofuran tosilate 0.5Kg, (1- (2- (trimethylsilyl) methylamino ethoxies
Base)) -1H- imidazoles -2- methylamine hydrochloride 1Kg, DMF 350Kg, react 10h, product warp at a temperature of 80 DEG C
Separate, be dried to obtain adsorbent product of the present invention.
2. the preparation of polyether modified silicon oil
By weight, by 100 parts of polyethers, 130 parts of containing hydrogen silicone oil, 2 parts of chloroplatinic acids, 18 parts of isopropanols, in nitrogen environment, 95 DEG C
At a temperature of react 4h, product obtains polyether modified silicon oil crude product, polyether modified silicon oil crude product is passed through through filtering, separation
In the chromatographic column of the adsorbent produced equipped with step 1, flow velocity 0.5BV obtains high-purity polyether modified silicon oil product.Product is compiled
Number M-1.
Embodiment 2
1. the preparation of adsorbent
In 1000L high-speed stirred kettles, the tertiary fourth of sepharose hydrophobic interaction medium 100Kg, 3- oxo aza ring butyl- 1- carboxylic acids is added
Ester 0.1Kg, (R)-(+) -3- amido tetrahydrofuran tosilate 0.1Kg, (1- (2- (trimethylsilyl) methylamino ethoxies
Base)) -1H- imidazoles -2- methylamine hydrochloride 0.5Kg, DMF 200Kg, 6h then is reacted at a temperature of 60 DEG C,
Product is through separating, being dried to obtain adsorbent product of the present invention.
2. the preparation of polyether modified silicon oil
By weight, by 100 parts of polyethers, 80 parts of containing hydrogen silicone oil, 1 part of chloroplatinic acid, 10 parts of isopropanols are in nitrogen environment, 80 DEG C of temperature
The lower reaction 2h of degree, product obtains polyether modified silicon oil crude product, polyether modified silicon oil crude product is passed through into dress through filtering, separation
Have in the chromatographic column of adsorbent of step 1 production, flow velocity 0.5BV obtains high-purity polyether modified silicon oil product.Production code member
M-2。
Embodiment 3
1. the preparation of adsorbent
In 1000L high-speed stirred kettles, the tertiary fourth of sepharose hydrophobic interaction medium 100Kg, 3- oxo aza ring butyl- 1- carboxylic acids is added
Ester 1Kg, (R)-(+) -3- amido tetrahydrofuran tosilate 1Kg, (1- (2- (trimethylsilyl) ethoxymethyl)) -
1H- imidazoles -2- methylamine hydrochloride 2Kg, DMF 500Kg, 15h, product warp are then reacted at a temperature of 100 DEG C again
Separate, be dried to obtain adsorbent product of the present invention.
2. the preparation of polyether modified silicon oil
By weight, by 100 parts of polyethers, 180 parts of containing hydrogen silicone oil, 5 parts of chloroplatinic acids, 30 parts of isopropanols, in nitrogen environment, 110
4h is reacted at a temperature of DEG C, product obtains polyether modified silicon oil crude product, polyether modified silicon oil crude product is led to through filtering, separation
In the chromatographic column for entering the adsorbent produced equipped with step 1, flow velocity 0.5BV obtains high-purity polyether modified silicon oil product.Product
Numbering M-3.
Comparative example 1
Step 1 is added without 3- oxo aza ring butyl- 1- carboxylic acid tert-butyl esters, other conditions be the same as Example 1.Production code member M-4.
Comparative example 2
Step 1 is added without (R)-(+) -3- amido tetrahydrofuran tosilate, other conditions be the same as Example 1.Production code member
M-5。
Comparative example 3
Step 1 is added without (1- (2- (trimethylsilyl) ethoxymethyl)) -1H- imidazoles -2- methylamine hydrochlorides, and other conditions are same
Embodiment 1.Production code member M-6.
Comparative example 4
The adsorbent product that the present invention is produced is added without, is adsorbed using the activated carbon of equivalent as adsorbent.Product is compiled
Number M-7.
Embodiment 4
The adsorbent product that embodiment 1-3 and comparative example 1-4 are produced loads chromatographic column, by the polyether-modified silicon of technical grade
Oil is adsorbed by chromatographic column, flow velocity 0.5BV, then examines the purity of polyether modified silicon oil product and by standard GB/
T16801-1997 examines it as performance during fabric antistatic additive, is shown in Table 1.
Table 1：The polyether modified silicon oil product purity produced through different process and the surface ratio applied to fabric after fabric
Resistance
| Production code member | Purity/% | Surface specific resistance/Ω |
| M-1 | 99.99 | 7.5·106 |
| M-2 | 99.99 | 7.7·106 |
| M-3 | 99.99 | 7.4·106 |
| M-4 | 99.77 | 2.1·107 |
| M-5 | 99.69 | 2.8·107 |
| M-6 | 99.74 | 2.3·107 |
| M-7 | 99.59 | 8.4·107 |
Claims (4)
1. a kind of preparation method of antistatic additive polyether modified silicon oil processed, it is characterised in that preparation method comprises the following steps：
By weight, by 100 parts of polyethers, 80-180 parts of containing hydrogen silicone oil, 1-5 parts of chloroplatinic acids, 10-30 parts of isopropanols, in nitrogen
Environment, 2-6h is reacted at a temperature of 80-110 DEG C, and product obtains polyether modified silicon oil crude product through filtering, separation, will be polyether-modified
Silicone oil crude product is passed through in the chromatographic column equipped with high-efficiency adsorbent, flow velocity 0.5BV, that is, obtains the production of high-purity polyether modified silicon oil
Product.
2. a kind of preparation method of antistatic additive polyether modified silicon oil processed according to claim 1, it is characterised in that institute
The preparation method for stating high-efficiency adsorbent comprises the following steps：
By weight, by 100 parts of sepharose hydrophobic interaction medium, 0.1-1 parts of 3- oxo aza ring butyl- 1- carboxylic acid tert-butyl esters,
(R)-(+) 0.1-1 parts of -3- amido tetrahydrofurans tosilate, (1- (2- (trimethylsilyl) ethoxymethyl)) -1H-
0.5-2 parts of imidazoles -2- methylamine hydrochlorides, are added in 200-500 parts of DMFs, then in 60-100 DEG C of temperature
Lower reaction 6-15h, product is dried through separation, obtains high-efficiency adsorbent.
3. a kind of preparation method of antistatic additive polyether modified silicon oil processed according to claim 2, it is characterised in that：Press
Parts by weight meter, (R)-(+) -3- amido tetrahydrofuran tosilate of addition obtains number for 0.1-0.5 parts.
4. a kind of preparation method of antistatic additive polyether modified silicon oil processed according to claim 2, it is characterised in that：Press
Parts by weight meter, the number of the 3- oxo aza ring butyl- 1- carboxylic acid tert-butyl esters of addition is 0.1-0.5 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710641129.4A CN107286348A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of antistatic additive polyether modified silicon oil processed |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710641129.4A CN107286348A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of antistatic additive polyether modified silicon oil processed |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107286348A true CN107286348A (en) | 2017-10-24 |
Family
ID=60104057
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710641129.4A Pending CN107286348A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of antistatic additive polyether modified silicon oil processed |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107286348A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116923A (en) * | 2020-01-03 | 2020-05-08 | 五色石新材料(杭州)有限公司 | Preparation method of polyether modified silicone oil |
| CN112574425A (en) * | 2020-12-07 | 2021-03-30 | 嘉兴联合化学有限公司 | Preparation and application of medical hydrophilic organic silicon oil |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040132951A1 (en) * | 2002-12-21 | 2004-07-08 | George Burkhart | Process for working up polyethersiloxanes |
| CN102961895A (en) * | 2011-11-17 | 2013-03-13 | 天津法莫西医药科技有限公司 | Preparation method of polyether modified polysiloxane defoaming agent |
| CN105949064A (en) * | 2016-05-27 | 2016-09-21 | 张玲 | Purification method of 1,2-cyclohexane diisononyl phthalate |
-
2017
- 2017-07-31 CN CN201710641129.4A patent/CN107286348A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040132951A1 (en) * | 2002-12-21 | 2004-07-08 | George Burkhart | Process for working up polyethersiloxanes |
| CN102961895A (en) * | 2011-11-17 | 2013-03-13 | 天津法莫西医药科技有限公司 | Preparation method of polyether modified polysiloxane defoaming agent |
| CN105949064A (en) * | 2016-05-27 | 2016-09-21 | 张玲 | Purification method of 1,2-cyclohexane diisononyl phthalate |
Non-Patent Citations (1)
| Title |
|---|
| 应国清等: "《药物分离工程》", 31 July 2011, 浙江大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116923A (en) * | 2020-01-03 | 2020-05-08 | 五色石新材料(杭州)有限公司 | Preparation method of polyether modified silicone oil |
| CN112574425A (en) * | 2020-12-07 | 2021-03-30 | 嘉兴联合化学有限公司 | Preparation and application of medical hydrophilic organic silicon oil |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109593464B (en) | Room-temperature-cured high-temperature-resistant organic silicon rubber coating, and preparation method and application thereof | |
| CN104592802B (en) | A kind of preparation method of organic silicon modified by polyether | |
| CN107286348A (en) | A kind of preparation method of antistatic additive polyether modified silicon oil processed | |
| CN104559727A (en) | Double-component polyurethane white glass finishing varnish and preparation method thereof | |
| CN110256677B (en) | Epoxy modified trifluoropropyl silicone oil and preparation method thereof | |
| CN101016383A (en) | Method of producing high boiling point silicon oil | |
| DE112005000098T5 (en) | High-resistant packing material for liquid chromatography | |
| CN112358619A (en) | Preparation method of methyl modified polysiloxane with adjustable viscosity | |
| CN104109244B (en) | A kind of long chain fluorine-containing alkyl-silicone oil and synthetic method thereof | |
| CN105801861B (en) | The method of organosilicon high-boiling product preparation superfines silicone resin | |
| CN102634031A (en) | Heat-resisting poly (silazane-siloxane) polymer and preparation method thereof | |
| CN107226909A (en) | A kind of fabric softener epoxy modified polysiloxane preparation method processed | |
| CN105384934A (en) | Preparation method of terminal hydrogen-containing silicone oil | |
| CN100471898C (en) | Method of preparing star-type multi-arm silicon oil | |
| EP1804965B1 (en) | Use of hydrophobized silica gel as a selective sorbent for removing organic silicon compounds | |
| WO2010149547A1 (en) | Method for producing dodeca halogen neopentasilanes | |
| CN102993225A (en) | Preparation method of anti-hydrolysis organosilane surfactant | |
| CN113429931A (en) | Addition type silk-screen silica gel and preparation method thereof | |
| CN107312177A (en) | A kind of preparation method of cutting fluid polyether modified silicon oil processed | |
| CN102875585A (en) | Method for preparing tetramethyl divinyl disiloxane | |
| CN110157331B (en) | Epoxy anticorrosive paint and preparation method thereof | |
| CN101942096B (en) | Modified amino silicone oil and preparation method thereof | |
| DE60205521T2 (en) | Process for the preparation of linear organohydrosiloxanes | |
| JP6644588B2 (en) | Composite particles, method for producing the same, and oil / water separation material | |
| CN108070087B (en) | Preparation method of fluorine-containing polyether modified organic silicon polyol |
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 | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20190918 Address after: Yiwu City, the new town hospital in Zhejiang province Jinhua city 5 District 322009 Building 1 unit 201 room Applicant after: Yiwu Ce New Material Co., Ltd. Address before: Yiwu City, the new town hospital in Zhejiang province Jinhua city 5 District 322009 Building 1 unit 201 room Applicant before: Wang Yi Lin |
|
| TA01 | Transfer of patent application right | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171024 |
|
| RJ01 | Rejection of invention patent application after publication |