CN115850711A - Washable hydrophilic darkening silicone oil and preparation method and finishing agent thereof - Google Patents
Washable hydrophilic darkening silicone oil and preparation method and finishing agent thereof Download PDFInfo
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- CN115850711A CN115850711A CN202211672583.3A CN202211672583A CN115850711A CN 115850711 A CN115850711 A CN 115850711A CN 202211672583 A CN202211672583 A CN 202211672583A CN 115850711 A CN115850711 A CN 115850711A
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Abstract
The invention discloses washable hydrophilic darkening silicone oil and a preparation method thereof, wherein the washable hydrophilic darkening silicone oil comprises a chain segment shown in a structural formula I:
wherein, m is more than or equal to 20 and more than or equal to 3; r 2 ＝
n≥5；
PO is propylene oxide, EO is ethylene oxide, c is more than or equal to 8 and more than or equal to 6, d is more than or equal to 5 and more than or equal to 2;
Description
Technical Field
The invention relates to the technical field of organic silicon, and particularly relates to washable hydrophilic darkening silicone oil, a preparation method thereof and a finishing agent.
Background
The fabric is dyed to be black, and the fabric generally comprises sulfur black cloth and active black cloth, wherein the sulfur black cloth is obtained by dyeing the fabric through sulfur black dye, and the active black cloth is obtained by dyeing the fabric through active dye. No matter the depth of the fabric dyed by the sulfur dye or the reactive dye has a certain limit, sometimes when the depth is required to be increased by 30 percent or 40 percent by customers, even if the using amount of the dye is increased, the color depth can not be further increased. At the moment, an auxiliary agent is needed, the depth can be reached after the sizing, the one-step forming is realized, the trouble of soaping for fixation after dyeing is avoided, and the water, the electricity and the time are saved. Most importantly, the depth which cannot be added with color is achieved. Therefore, the development of the silicone oil auxiliary agent solves the hand feeling problem of the fabric and the depth problem of color. However, the existing deepening silicone oil is not hydrophilic and has very poor stability, and even though some enterprises develop the hydrophilic deepening silicone oil, the washing resistance is also general, so that the development of the washing-resistant hydrophilic deepening silicone oil is needed to solve the current situation.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide washable hydrophilic deepening silicone oil which can improve the depth of textile cloth, reduce the using amount of reactive dyes and save enterprise cost, and after the textile is subjected to after-treatment by using a finishing agent of the silicone oil, the textile has excellent hydrophilicity and washing resistance.
In order to achieve the purpose, the invention provides washable hydrophilic deepening silicone oil which comprises a chain segment shown in a structural formula I:
wherein, m is more than or equal to 20 and more than or equal to 3;
Correspondingly, the invention also provides a preparation method of the washable hydrophilic darkening silicone oil, which comprises the following preparation steps:
(1) Reacting octamethyltetrasiloxane and a hydrogen-containing double-end socket at 30-45 ℃ under the condition of concentrated sulfuric acid serving as a catalyst to prepare an intermediate;
(2) Reacting the intermediate with allyl epoxy polyether under the condition of chloroplatinic acid catalyst to obtain diepoxy terminated polyether silicone oil;
(3) Reacting diepoxy terminated polyether silicone oil, tetramethyl ethylenediamine and secondary aminated polyether amine in a weak acid condition in a downward way to prepare washable hydrophilic deepening silicone oil.
In some embodiments, in step (1), the mass ratio of octamethyltetrasiloxane to hydrogen-containing double head is from 100.
In some embodiments, in step (2), the mass ratio of intermediate to allyl epoxy polyether is 5.
In some embodiments, the reaction temperature in step (2) is less than 85 ℃, preferably less than 85 ℃, and more preferably 75 to 80 ℃.
In some embodiments, in step (3), the mild acid conditions are selected from at least one of acetic acid, propionic acid, lauric acid, isopropanol.
In some embodiments, in step (3), the secondary aminated polyetheramine has a weight average molecular weight of 500-2500. Illustratively, the secondary aminated polyetheramine can have a weight average molecular weight of, but not limited to, 500, 1000, 1500, 2000, 2500, specifically, the secondary aminated polyetheramine is selected from the group consisting of polyetheramine M-600, polyetheramine M-1000, polyetheramine M-2005, but not limited thereto.
In some embodiments, in step (3), the mass ratio of diepoxy terminated polyether silicone oil to secondary aminated polyether amine is 100: 120-140.
In some embodiments, the reaction temperature in step (3) is 70-90 ℃, and illustratively, the temperature may be, but is not limited to, 70 ℃, 72 ℃, 74 ℃, 76 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃, and preferably 85 ℃.
In some embodiments, the allyl epoxy polyether has the following structural formula:
wherein PO is propylene oxide, EO is ethylene oxide, a is more than or equal to 30 and more than or equal to 5, and b is more than or equal to 20 and more than or equal to 6.
In some embodiments, the allyl epoxy polyether has a molecular weight of 500 to 2000. The molecular weight of the allyl epoxy polyether can be, but is not limited to, 500, 1000, 1500, 2000, and specifically, the allyl epoxy polyether is selected from APE1000, APE600, APE1500, APEG-1000, but not limited thereto.
Wherein, the reaction mechanism is as follows:
step (1):
step (2):
wherein the content of the first and second substances,
and (3):
wherein the content of the first and second substances,
simplified to
In some embodiments, the wash-resistant hydrophilic darkening silicone oil has the following structural formula:
wherein 20. Gtoreq.m.gtoreq.3, preferably 12. Gtoreq.m.gtoreq.3.
In some embodiments, the wash-resistant hydrophilic darkening silicone oil has the following structural formula:
wherein 20. Gtoreq.m.gtoreq.3, preferably 12. Gtoreq.m.gtoreq.3.
Correspondingly, the invention also provides a finishing agent which comprises, by weight, 10-30 parts of washable hydrophilic darkening silicone oil, 5-15 parts of an emulsifier, 2-10 parts of acetic acid and 100 parts of water. Illustratively, the emulsifier can be, but is not limited to, an AEO-3 emulsifier, an AEO-9 emulsifier.
The invention has the following beneficial effects:
the washable hydrophilic deepening silicone oil contains more ethylene oxide, can improve the hydrophilicity of textile cloth, also contains more propylene oxide, can improve the hand feeling of the textile cloth, particularly contains two polyether amine structures with different properties to react, partially carries out polyamine reaction, retains part of H in secondary amine, can react with hydroxyl on the surface of cotton fibers, can also obtain N lone electron pairs, and combines the H in emulsion after the emulsion is emulsified + And when the finishing is carried out, the finishing agent can react with hydroxyl on the surface of the cotton fiber, so that the binding force is too high, and the water washing resistance of the textile fabric is greatly improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of washable hydrophilic darkening silicone oil comprises the following preparation steps:
(1) Sequentially adding 100g of octamethyltetrasiloxane and 1g of hydrogen-containing double-end socket into a reaction bottle, adding a proper amount of concentrated sulfuric acid as a catalyst, and reacting at the temperature of 40 ℃ for 24 hours to obtain an intermediate;
(2) Adding 50g of the intermediate and 10g of allyl epoxy polyether APEG-1000 into a reaction bottle, adding isopropanol, heating to 80 ℃, adding chloroplatinic acid, preserving heat for 1 hour, heating to 80 ℃, and preserving heat for reaction for 6 hours to obtain diepoxy terminated polyether silicone oil;
(4) And sequentially adding 100g of diepoxy terminated polyether silicone oil, 120g of tetramethylethylenediamine and 130g of polyetheramine M-600 into a reaction bottle, adding a proper amount of isopropanol, stirring for 20 minutes, slowly heating to 85 ℃, reacting for 8 hours in a reflux state, cooling and discharging, wherein the product is washable hydrophilic deepened silicone oil.
Example 2
A preparation method of washable hydrophilic darkening silicone oil comprises the following preparation steps:
(1) Sequentially adding 100g of octamethyltetrasiloxane and 1.5g of hydrogen-containing double-end socket into a reaction bottle, adding a proper amount of concentrated sulfuric acid as a catalyst, and reacting at the temperature of 40 ℃ for 24 hours to obtain an intermediate;
(2) Adding 50g of the intermediate and 10g of allyl epoxy polyether APE600 into a reaction bottle, adding isopropanol, heating to 80 ℃, adding chloroplatinic acid, preserving heat for 2 hours, heating to 100 ℃, and preserving heat for reaction for 8 hours to obtain diepoxy terminated polyether silicone oil;
(4) Sequentially adding 100g of diepoxy terminated polyether silicone oil, 130g of tetramethylethylenediamine and 120g of polyether amine M-1000 into a reaction bottle, adding a proper amount of glacial acetic acid and isopropanol, stirring for 30 minutes, slowly heating to 85 ℃, reacting for 10 hours in a reflux state, cooling and discharging, wherein the product is washable hydrophilic deepening silicone oil.
Example 3
A preparation method of washable hydrophilic deepening silicone oil comprises the following preparation steps:
(1) Sequentially adding 100g of octamethyltetrasiloxane and 2g of hydrogen-containing double-end socket into a reaction bottle, adding a proper amount of concentrated sulfuric acid as a catalyst, and reacting at the temperature of 35 ℃ for 24 hours to obtain an intermediate;
(2) Adding 50g of the intermediate and 10g of allyl epoxy polyether APE1000 into a reaction bottle, adding isopropanol, heating to 80 ℃, adding chloroplatinic acid as a catalyst, preserving heat for 2 hours, heating to 100 ℃, and preserving heat for reaction for 8 hours to obtain diepoxy terminated polyether silicone oil;
(4) And sequentially adding 100g of diepoxy terminated polyether silicone oil, 140g of tetramethylethylenediamine and 140g of polyetheramine M-2005 into a reaction bottle, adding a proper amount of glacial acetic acid and isopropanol, stirring for 30 minutes, slowly heating to 85 ℃, reacting for 10 hours in a reflux state, cooling and discharging, wherein the product is washable hydrophilic deepening silicone oil.
Example 4
A finishing agent comprises, by weight, 10 parts of washable hydrophilic darkening silicone oil, 5 parts of AEO-3 emulsifier, 4 parts of acetic acid and 100 parts of water;
washable hydrophilic darkening silicone oil was prepared by example 1;
the preparation method comprises the following steps: mixing AEO-3 emulsifier with washable hydrophilic deepening silicone oil, stirring, and adding acetic acid and water to obtain the finishing agent.
Example 5
A finishing agent comprises, by weight, 20 parts of washable hydrophilic deepening silicone oil, 20 parts of AEO-9 emulsifier, 6 parts of acetic acid and 100 parts of water;
wash-resistant hydrophilic darkening silicone oil was prepared by example 2;
the preparation method comprises the following steps: mixing the AEO-9 emulsifier with the washable hydrophilic darkening silicone oil, uniformly stirring, and adding acetic acid and water to prepare the finishing agent.
Example 6
A finishing agent comprises 15 parts by weight of washable hydrophilic darkening silicone oil, 5 parts by weight of AEO-9 emulsifier, 5 parts by weight of acetic acid and 100 parts by weight of water;
wash-resistant hydrophilic darkening silicone oil was prepared by example 3;
the preparation method comprises the following steps: mixing AEO-9 emulsifier with washable hydrophilic deepening silicone oil, stirring, and adding acetic acid and water to obtain the finishing agent.
The finishing agents prepared in examples 4 to 6 were subjected to a post-finishing process, and the treated active black cloths (specification 10 cm. Times.20 cm) were finished with the above finishing agents, and then subjected to appearance observation and a hydrophilicity test with a blank control which was not finished.
Appearance observation, namely observing whether the color of the treated active black cloth is deepened or not by naked eyes;
hydrophilicity was determined by dropping 1 drop of water from a position 1cm from the fabric using a standard dropper (25 drops/mL) using a static drip method, and determining the hydrophilicity as the time for which the drop of water was completely absorbed. The shorter the time, the better the hydrophilicity.
TABLE 1 test results
From the test results in table 1, it can be seen that the blank control active black cloth is almost not hydrophilic, and the hydrophilicity is greatly improved and the color is further darkened by the fabric after the post-finishing by the washable hydrophilic darkening silicone oil in the invention examples 1-3, and further it can be seen that the decrease in hydrophilicity is small after 5 times of washing, which indicates that the adhesive force of the finishing agent of the invention and the textile is good, and the good washing resistance can be realized.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The washable hydrophilic deepening silicone oil is characterized by comprising a chain segment shown in a structural formula I:
wherein, m is more than or equal to 20 and more than or equal to 3;
2. The wash-resistant hydrophilic darkening silicone oil of claim 1, wherein the wash-resistant hydrophilic darkening silicone oil has the following structural formula:
3. the wash-resistant hydrophilic darkening silicone oil of claim 1 wherein the structural formula of the wash-resistant hydrophilic darkening silicone oil is as follows:
4. a method for preparing wash-resistant hydrophilic darkening silicone oil according to claim 1, characterized in that the preparation step comprises:
(1) Reacting octamethyltetrasiloxane and a hydrogen-containing double-end socket at 30-45 ℃ under the condition of concentrated sulfuric acid serving as a catalyst to prepare an intermediate;
(2) Reacting the intermediate with allyl epoxy polyether under the condition of chloroplatinic acid catalyst to obtain diepoxy terminated polyether silicone oil;
(3) Reacting diepoxy terminated polyether silicone oil, tetramethyl ethylenediamine and secondary aminated polyether amine in a weak acid condition in a downward way to prepare washable hydrophilic deepening silicone oil.
5. The method for preparing washable hydrophilic deepening silicone oil according to claim 4, wherein in the step (1), the mass ratio of octamethyltetrasiloxane to hydrogen-containing double end enclosure is 100.
6. The method for preparing washable hydrophilic darkening silicone oil according to claim 4, wherein in the step (2), the mass ratio of the intermediate to the allyl epoxy polyether is 5.
7. The method for preparing wash-resistant hydrophilic thickening silicone oil according to claim 4, wherein in step (3), the secondary aminated polyetheramine has a molecular weight of 500-2500.
8. The method for preparing washable hydrophilic deepening silicone oil according to claim 4, wherein in the step (3), the mass ratio of the diepoxy terminated polyether silicone oil to the secondary aminated polyether amine is 100: 120-140.
9. The method for preparing wash-resistant hydrophilic darkening silicone oil of claim 4, wherein in step (2), the allyl epoxy polyether has a molecular weight of 500 to 2000.
10. A finish, characterized by comprising, in parts by weight, 10 to 30 parts of the wash-resistant hydrophilic darkening silicone oil of any of claims 1 to 3, 5 to 15 parts of an emulsifier, 2 to 10 parts of acetic acid, and 100 parts of water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117720733A (en) * | 2023-12-18 | 2024-03-19 | 江南大学 | Quaternary ammonium amino polyether modified silicone oil and solvent-free synthesis method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106693829A (en) * | 2016-12-29 | 2017-05-24 | 柏青龙 | Modified composite type surface active agent |
| CN107383374A (en) * | 2017-08-30 | 2017-11-24 | 嘉兴固高日化有限公司 | A kind of preparation method of bafta hydrophilic softening agent |
| CN110409188A (en) * | 2019-08-06 | 2019-11-05 | 广东科峰新材料科技有限公司 | A kind of hydrophilic soft finishing agent of cotton fabric and preparation method thereof |
| CN113373696A (en) * | 2021-06-18 | 2021-09-10 | 广东宏昊化工有限公司 | Softening agent for bamboo fiber fabric and preparation method thereof |
| CN114000355A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Hydrophilic elastic silicone oil finishing agent for pure cotton fabric and preparation method thereof |
| CN114517411A (en) * | 2022-01-27 | 2022-05-20 | 浙江传化功能新材料有限公司 | Preparation method and application of washable cotton fabric softener |
-
2022
- 2022-12-23 CN CN202211672583.3A patent/CN115850711A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106693829A (en) * | 2016-12-29 | 2017-05-24 | 柏青龙 | Modified composite type surface active agent |
| CN107383374A (en) * | 2017-08-30 | 2017-11-24 | 嘉兴固高日化有限公司 | A kind of preparation method of bafta hydrophilic softening agent |
| CN110409188A (en) * | 2019-08-06 | 2019-11-05 | 广东科峰新材料科技有限公司 | A kind of hydrophilic soft finishing agent of cotton fabric and preparation method thereof |
| CN113373696A (en) * | 2021-06-18 | 2021-09-10 | 广东宏昊化工有限公司 | Softening agent for bamboo fiber fabric and preparation method thereof |
| CN114000355A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Hydrophilic elastic silicone oil finishing agent for pure cotton fabric and preparation method thereof |
| CN114517411A (en) * | 2022-01-27 | 2022-05-20 | 浙江传化功能新材料有限公司 | Preparation method and application of washable cotton fabric softener |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117720733A (en) * | 2023-12-18 | 2024-03-19 | 江南大学 | Quaternary ammonium amino polyether modified silicone oil and solvent-free synthesis method thereof |
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