CN109627445B - Preparation method of straight-chain tertiary amine type block amino silicone oil - Google Patents
Preparation method of straight-chain tertiary amine type block amino silicone oil Download PDFInfo
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- 229920013822 aminosilicone Polymers 0.000 title claims abstract description 49
- 150000003512 tertiary amines Chemical class 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920002545 silicone oil Polymers 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000004593 Epoxy Substances 0.000 claims abstract description 12
- 239000012970 tertiary amine catalyst Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 36
- -1 siloxane ring Chemical group 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 150000001412 amines Chemical group 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 6
- 238000004383 yellowing Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 4
- 238000007730 finishing process Methods 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 150000002431 hydrogen Chemical class 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 125000003700 epoxy group Chemical group 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 229960000583 acetic acid Drugs 0.000 description 6
- 239000012362 glacial acetic acid Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229920000570 polyether Polymers 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002759 woven fabric Substances 0.000 description 2
- CIPOCPJRYUFXLL-UHFFFAOYSA-N 2,3,4-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC=C(O)C(CN(C)C)=C1CN(C)C CIPOCPJRYUFXLL-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
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
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
-
- 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
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of straight-chain tertiary amine type block amino silicone oil, which comprises the following steps: (1) reacting first double-end oxidation silicone oil with the number of siloxy links of 50-100 with methylethanolamine to generate hydroxyl-end straight-chain tertiary amine amino silicone oil; (2) and (2) carrying out ultrasonic reaction on the terminal hydroxyl straight-chain tertiary amine type amino silicone oil prepared in the step (1) and second double-terminal epoxy silicone oil with the number of silicone-oxygen chain links of 1-5 in the presence of a tertiary amine catalyst to generate straight-chain tertiary amine type block amino silicone oil. The straight-chain tertiary amine type block amino silicone oil prepared by the method has no active hydrogen, so that the phenomena of yellowing and color change caused in the storage and use processes are avoided; and in the whole preparation process, no organic solvent is used, the washing fastness is improved, the environmental protection pressure is reduced, and the use amount of the block silicone oil for achieving the same hand feeling is less than that of the conventional block silicone oil in the after-finishing process of the textile.
Description
Technical Field
The invention relates to a preparation method of straight-chain tertiary amine type block amino silicone oil.
Background
At present, the types of organic silicon used in the textile after-finishing market mainly comprise 2 types, namely amino silicone oil and block silicone oil. These 2 major classes of afterfinish aids each have advantages and also suffer from the following disadvantages: one, amino silicone oil: firstly, the emulsion has poor stability, secondly, the compatibility is poor, and thirdly, the finished textile is hydrophobic and has static electricity; and fourthly, the yellowing and the color change of the fabric are easily caused. Diblock silicone oil: the washing fastness is not good, the washing agent contains solvent, and the block silicone oil has no effect on natural fiber compared with amino silicone oil, and the using amount is large.
In order to overcome the application defects of amino silicone oil and block silicone oil, the method generally adopted is as follows: grafting polyether hydrophilic groups on branched chains of amino silicone oil to seal active hydrogen on amino groups, improving yellowing and color change, and improving hydrophilicity and antistatic property, but causing the reduction of a softening effect; when the block silicone oil is prepared, a low-solvent or solvent-free manufacturing process is adopted, but the raw materials and conditions of the synthesis process are more limited, and the obtained product has a use effect which is not as good as that of the original block silicone oil.
Disclosure of Invention
In view of the above-mentioned disadvantages, the present invention aims to provide a method for preparing a linear tertiary amine type block amino silicone oil.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme: a preparation method of linear tertiary amine type block amino silicone oil comprises the following steps:
(1) preparation of hydroxyl-terminated straight-chain tertiary amine type amino silicone oil: mixing and reacting a first double-terminal epoxy group silicone oil raw material and methyl ethanolamine raw material according to a molar ratio of 1: 2-2.2 to generate a linear chain tertiary amine amino silicone oil; wherein the reaction equation is as follows:
(2) preparation of straight-chain tertiary amine type block amino silicone oil: taking the hydroxyl-terminated linear tertiary amine type amino silicone oil obtained in the step (1) as a raw material, adding a second double-terminal epoxy silicone oil and a tertiary amine catalyst as raw materials, and carrying out ultrasonic reaction to generate linear tertiary amine type block amino silicone oil; wherein, the reaction equation is as follows:
wherein X is represented by-CH2CH2CH2OCH2-，a＝50～100，a1＝1～5，b≥1。
In the above technical solution, preferably, in the step (1), the reaction conditions for preparing the hydroxyl-terminated linear tertiary amine type amino silicone oil are as follows: controlling the reaction temperature at 75-80 ℃, and carrying out ultrasonic stirring reaction for 2-4 hours with the ultrasonic power of 40-60 watts.
In the above technical solution, preferably, in the step (1), the raw material of the first epoxy-terminated silicone oil and the raw material of the methylethanolamine are pretreated, specifically: vacuumizing at the temperature of 105-110 ℃, stirring for 1-3 hours under the vacuum degree of-0.01-0.03 MPa, and removing the dimethyl siloxane ring body and water remained in the raw material.
In the above technical solution, preferably, in the step (2), the reaction conditions for preparing the linear tertiary amine type block aminosilicone oil are as follows: the temperature is controlled to be 110-130 ℃, the ultrasonic stirring reaction is carried out for 4-6 hours, and the ultrasonic power is 100-200 watts.
In the above technical solution, in the step (2), the amount of the tertiary amine catalyst is preferably 0.1 to 5% of the total weight of the raw material second double-terminal epoxy silicone oil and the raw material hydroxyl-terminal straight-chain tertiary amine type amino silicone oil. .
In the above technical solution, preferably, the tertiary amine catalyst is one or a mixture of two or more of N- (γ' -dimethylaminopropyl) - γ -aminopropylmethyldimethoxysilane, dimethyldodecyl tertiary amine, and tris- (dimethylaminomethyl) phenol.
Compared with the prior art, the invention has the following beneficial effects: 1) the straight-chain tertiary amine type block amino silicone oil prepared according to the invention has no active hydrogen, and the phenomena of yellowing and color change caused in the storage and use processes are avoided; 2) according to the process for preparing the linear-chain tertiary amine type block amino silicone oil, an organic solvent is not used, the washing fastness is improved, and the environmental protection pressure is reduced; 3) the proportion of the linear tertiary amine type block amino silicone oil hydrophilic polyether group prepared according to the invention is smaller, and the use amount of the linear tertiary amine type block amino silicone oil hydrophilic polyether group reaching the same hand feeling is less than that of the conventional block silicone oil in the after-finishing process of textiles.
Detailed Description
In order to explain the technical solution, the achieved objects and the effects of the present invention in detail, several embodiments will be enumerated below.
In the various embodiments described below, it is preferred that,
example 1
A first epoxy-terminated silicone oil (chemical formula is
The following examples are the same) and methyl ethanolamine raw materials are pretreated, specifically: vacuumizing at 105-110 ℃, controlling the vacuum degree at-0.01 to-0.03 MPa, stirring for 2 hours, and removing the dimethyl siloxane ring body and the water remained in the raw material.
136.6 g of first epoxy terminated silicone oil with the siloxane chain segment a of 50 and 3.02 g of methylethanolamine are weighed, added into a 500 ml four-neck reaction flask, put into an ultrasonic machine, heated and stirred, the temperature is controlled to be 75-80 ℃, the ultrasonic power is 40 watts, and the reaction is carried out for 2 hours.
Adding siloxane chain segment a1A second epoxy-terminated silicone oil of formula 1
The following examples are the same as above), 7.24 g of N- (γ '-dimethylaminopropyl) - γ -aminopropylmethyldimethoxysilane is added, 1.5 g of N- (γ' -dimethylaminopropyl) - γ -aminopropylmethyldimethoxysilane is added, the temperature is raised to 110 ℃, the ultrasonic power is 100 watts, the mixture is stirred and reacted for 6 hours, 1 g of glacial acetic acid is added, and the mixture is stirred for 30 minutes, so that the linear tertiary amine type block amino silicone oil is obtained.
Example 2
The method comprises the following steps of pretreating a first double-end epoxy group silicone oil raw material and methyl ethanolamine raw material: vacuumizing at 105-110 ℃, controlling the vacuum degree to be-0.01-0.03 MPa, stirring for 2 hours, and removing the dimethyl siloxane ring body and the water remained in the raw material.
136.6 g of first epoxy terminated silicone oil with the siloxane chain segment a of 50 and 3.02 g of methylethanolamine are weighed, added into a 500 ml four-neck reaction flask, put into an ultrasonic machine, heated and stirred, the temperature is controlled to be 75-80 ℃, the ultrasonic power is 40 watts, and the reaction is carried out for 2 hours.
Adding siloxane chain segment a1Adding 17.8 g of second double-terminal epoxy group silicone oil of 5, adding 1 g of N- (gamma' -dimethylaminopropyl) -gamma-aminopropyl methyl dimethoxysilane and 1 g of tri- (dimethylaminomethyl) phenol, heating to 110 ℃, enabling the ultrasonic power to be 100 watts, stirring for reacting for 6 hours, adding 1 g of glacial acetic acid, and stirring for 30 minutes to obtain the linear chain tertiary amine type block amino silicone oil.
Example 3
The method comprises the following steps of pretreating a first double-end epoxy group silicone oil raw material and methyl ethanolamine raw material: vacuumizing at the temperature of 105-110 ℃, stirring for 2 hours under the vacuum degree of-0.01-0.03 MPa, and removing the dimethyl siloxane ring body and the water remained in the raw materials.
189.4 g of first dual-end epoxy silicone oil with siloxane chain segment a of 70 and 3.02 g of methylethanolamine are weighed, added into a 500 ml four-neck reaction flask, put into an ultrasonic machine, heated and stirred, the temperature is controlled to be 75-80 ℃, the ultrasonic power is 40 watts, and the reaction is carried out for 3 hours.
Adding siloxane chain segment a1Adding 7.24 g of second epoxy-terminated silicone oil of 1, adding 2.5 g of N- (gamma' -dimethylaminopropyl) -gamma-aminopropylmethyldimethoxysilane, heating to 110 ℃, enabling ultrasonic power to be 100 watts, stirring for reacting for 6 hours, adding 1 g of glacial acetic acid, and stirring for 30 minutes to obtain the linear tertiary amine type blocked amino silicone oil.
Example 4
The method comprises the following steps of pretreating a first double-end epoxy group silicone oil raw material and methyl ethanolamine raw material: vacuumizing at the temperature of 105-110 ℃, stirring for 2 hours under the vacuum degree of-0.01-0.03 MPa, and removing the dimethyl siloxane ring body and the water remained in the raw materials.
189.4 g of first dual-end epoxy silicone oil with siloxane chain segment a of 70 and 3.02 g of methylethanolamine are weighed, added into a 500 ml four-neck reaction flask, put into an ultrasonic machine, heated and stirred, the temperature is controlled to be 75-80 ℃, the ultrasonic power is 40 watts, and the reaction is carried out for 3 hours.
Adding siloxane chain segment a117.8 g of second double-terminal epoxy group silicone oil of 5, 4 g of tris- (dimethylaminomethyl) phenol is added, the temperature is raised to 120 ℃, the ultrasonic power is 150 watts, the stirring reaction is carried out for 6 hours, 1 g of glacial acetic acid is added, and the stirring is carried out for 30 minutes, so as to obtain the straight-chain tertiary amine type block amino silicone oil.
Example 5
The method comprises the following steps of pretreating a first double-end epoxy group silicone oil raw material and methyl ethanolamine raw material: vacuumizing at the temperature of 105-110 ℃, stirring for 2 hours under the vacuum degree of-0.01-0.03 MPa, and removing the dimethyl siloxane ring body and the water remained in the raw materials.
268.6 g of first epoxy terminated silicone oil with siloxane chain segment a of 100 and 3.02 g of methylethanolamine are weighed, added into a 500 ml four-neck reaction flask, put into an ultrasonic machine, heated and stirred, the temperature is controlled to be 75-80 ℃, the ultrasonic power is 60 watts, and the reaction is carried out for 4 hours.
Adding siloxane chain segment a17.24 grams of second epoxy-terminated silicone oil of 1, N- (γ' -dimethylamino) was added2.5 g of propyl) -gamma-aminopropyl methyl dimethoxysilane and 3.5 g of tris- (dimethylaminomethyl) phenol are heated to 120 ℃, the ultrasonic power is 150 watts, the mixture is stirred and reacted for 6 hours, 1 g of glacial acetic acid is added, and the mixture is stirred for 30 minutes. Obtaining the straight-chain tertiary amine block amino silicone oil.
Example 6
The method comprises the following steps of pretreating a first double-end epoxy group silicone oil raw material and methyl ethanolamine raw material: vacuumizing at the temperature of 105-110 ℃, stirring for 2 hours under the vacuum degree of-0.01-0.03 MPa, and removing the dimethyl siloxane ring body and the water remained in the raw materials.
268.6 g of first epoxy terminated silicone oil with siloxane chain segment a of 100 and 3.02 g of methylethanolamine are weighed, added into a 500 ml four-neck reaction flask, put into an ultrasonic machine, heated and stirred, the temperature is controlled to be 75-80 ℃, the ultrasonic power is 60 watts, and the reaction is carried out for 4 hours
Adding siloxane chain segment a1Adding 17.8 g of second double-terminal epoxy silicone oil of 5, adding 3 g of tris- (dimethylaminomethyl) phenol, 3 g of dimethyldodecyl tertiary amine and 4 g of N- (gamma' -dimethylaminopropyl) -gamma-aminopropyl methyldimethoxysilane, heating to 130 ℃, controlling the ultrasonic power at 200 watts, stirring for reacting for 6 hours, adding 1 g of glacial acetic acid, and stirring for 30 minutes to obtain the linear tertiary amine type block amino silicone oil.
The following performance tests were performed on the linear tertiary amine block amino silicone oil prepared by the method selected from the above examples in 3 examples, specifically as follows:
the linear tertiary amine type block amino silicone oil prepared in example 1 emulsified into a softening finish with a solid content of 20%, designated as sample-1 the linear tertiary amine type block amino silicone oil prepared in example 3, emulsified into a softening finish with a solid content of 20%, designated as sample-2 the linear tertiary amine type block amino silicone oil prepared in example 6, emulsified into a softening finish with a solid content of 20%, designated as sample-3 the conventional amino silicone oil, emulsified into a softening finish with a solid content of 20%, designated as sample-4
Conventional block silicone oil emulsified into a soft finish with 20% solids, sample-5
Textile materials for experiments: pure cotton white woven fabric, pure polyester white woven fabric,
the finishing process comprises the following steps: preparing working solution 40 g/L, padding, drying at 95-105 ℃, and shaping at 150-160 ℃ for 60 seconds.
The test contents are as follows:
and (3) evaluation of softening effect: the test is touched by human hands, 5 persons/group, and the test is divided into 1-5 grades, the worst grade 1, and the best yellowing test grade 5: reference is made to GB/T8424.2-2001 textile color fastness test relative whiteness instrument evaluation method.
And (3) determining washing fastness: the test is carried out with reference to GB/T3921.1-1997 colour fastness to washing of the textile colour fastness test.
The performance test of the straight-chain tertiary amine type block amino silicone oil is shown in Table 1
TABLE 1 Performance test results for straight-chain tertiary amine type block amino silicone oils
The specific embodiments are only for explaining the present invention, and the present invention is not limited thereto, and those skilled in the art can make modifications without inventive contribution to the present embodiments as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (6)
1. The preparation method of the linear tertiary amine type block amino silicone oil is characterized by comprising the following steps:
(1) preparation of hydroxyl-terminated straight-chain tertiary amine type amino silicone oil: mixing and reacting a first double-terminal epoxy silicone oil raw material and methyl ethanolamine raw material according to a molar ratio of 1: 2-2.2 to generate a hydroxyl-terminal straight-chain tertiary amine amino silicone oil; wherein the reaction equation is as follows:
(2) preparation of straight-chain tertiary amine type block amino silicone oil: taking the hydroxyl-terminated linear tertiary amine type amino silicone oil generated in the step (1) as a raw material, adding a second double-terminal epoxy silicone oil and a tertiary amine catalyst as raw materials, and carrying out ultrasonic reaction to generate linear tertiary amine type block amino silicone oil; wherein, the reaction equation is as follows:
wherein X is-CH2CH2CH2OCH2-，a＝50～100，a1＝1～5，b≥1。
2. The method according to claim 1, wherein in the step (1), the reaction conditions for preparing the hydroxyl-terminated linear tertiary amine type amino silicone oil are as follows: controlling the reaction temperature at 75-80 ℃, carrying out ultrasonic stirring reaction for 2-4 hours, and controlling the ultrasonic power at 40-60W.
3. The method according to claim 1 or 2, wherein in the step (1), the raw material of the first epoxy-terminated silicone oil and the raw material of the methylethanolamine are subjected to pretreatment, specifically: vacuumizing at the temperature of 105-110 ℃, stirring for 1-3 hours under the vacuum degree of-0.01-0.03 MPa, and removing the dimethyl siloxane ring body and water remained in the raw material.
4. The method according to claim 1, wherein the reaction conditions for preparing the linear tertiary amine block aminosilicone oil in the step (2) are as follows: the temperature is controlled to be 110-130 ℃, the ultrasonic stirring reaction is carried out for 4-6 hours, and the ultrasonic power is 100-200 watts.
5. The method according to claim 1, wherein in the step (2), the tertiary amine catalyst is used in an amount of 0.1 to 5% by weight based on the total amount of the raw material hydroxyl-terminated linear tertiary amine-type amino silicone oil and the raw material second terminal epoxy-type silicone oil.
6. The method according to claim 1 or 5, wherein the tertiary amine catalyst is one or a mixture of two or more of N- (γ' -dimethylaminopropyl) - γ -aminopropylmethyldimethoxysilane, dimethyldodecyltertiary amine, and tris- (dimethylaminomethyl) phenol.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007024792A1 (en) * | 2005-08-25 | 2007-03-01 | Henkel Corporation | Rtv silicone compositions using carbamate functional alpha silane crosslinkers |
| CN102504260A (en) * | 2011-11-07 | 2012-06-20 | 邬元娟 | Method for synthesizing dihydroxyl-terminated polysiloxane |
| CN107820527A (en) * | 2015-05-26 | 2018-03-20 | 鲁道夫有限公司 | Polyurethane organopolysiloxane |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007024792A1 (en) * | 2005-08-25 | 2007-03-01 | Henkel Corporation | Rtv silicone compositions using carbamate functional alpha silane crosslinkers |
| CN102504260A (en) * | 2011-11-07 | 2012-06-20 | 邬元娟 | Method for synthesizing dihydroxyl-terminated polysiloxane |
| CN107820527A (en) * | 2015-05-26 | 2018-03-20 | 鲁道夫有限公司 | Polyurethane organopolysiloxane |
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