CN115772266B - Low-VOC silicone oil and preparation method thereof - Google Patents
Low-VOC silicone oil and preparation method thereof Download PDFInfo
- Publication number
- CN115772266B CN115772266B CN202211691596.5A CN202211691596A CN115772266B CN 115772266 B CN115772266 B CN 115772266B CN 202211691596 A CN202211691596 A CN 202211691596A CN 115772266 B CN115772266 B CN 115772266B
- Authority
- CN
- China
- Prior art keywords
- silicone oil
- low
- hydrogen
- voc
- molecular weight
- 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.)
- Active
Links
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 42
- 239000001257 hydrogen Substances 0.000 claims abstract description 42
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 33
- 229920000570 polyether Polymers 0.000 claims abstract description 33
- 239000004593 Epoxy Substances 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 150000001412 amines Chemical class 0.000 claims abstract description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 13
- NRTJGTSOTDBPDE-UHFFFAOYSA-N [dimethyl(methylsilyloxy)silyl]oxy-dimethyl-trimethylsilyloxysilane Chemical compound C[SiH2]O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C NRTJGTSOTDBPDE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 14
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- -1 bis-dimethylamino ethyl Chemical group 0.000 claims description 2
- ZISSAWUMDACLOM-UHFFFAOYSA-N triptane Chemical compound CC(C)C(C)(C)C ZISSAWUMDACLOM-UHFFFAOYSA-N 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 10
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000012855 volatile organic compound Substances 0.000 description 29
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 13
- 239000000523 sample Substances 0.000 description 13
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 5
- JUXXCHAGQCBNTI-UHFFFAOYSA-N 1-n,1-n,2-n,2-n-tetramethylpropane-1,2-diamine Chemical compound CN(C)C(C)CN(C)C JUXXCHAGQCBNTI-UHFFFAOYSA-N 0.000 description 4
- 229920013822 aminosilicone Polymers 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 125000000746 allylic group Chemical group 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000009958 sewing Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920006027 ternary co-polymer Polymers 0.000 description 1
- 150000003512 tertiary amines Chemical group 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Silicon Polymers (AREA)
Abstract
The invention discloses a low VOC silicone oil and a preparation method thereof, comprising the following steps: (1) Mixing octamethyltetrasiloxane with hydrogen-containing double seal heads, adding concentrated sulfuric acid, and reacting at 30-45 ℃ to obtain hydrogen-containing silicone oil; (2) Adding sodium carbonate into the hydrogen-containing silicone oil at the end for neutralization, filtering, and then carrying out vacuumizing treatment at high temperature to obtain the hydrogen-containing silicone oil at the end of the low ring body; (3) Mixing the low-ring-end hydrogen-containing silicone oil with the molecular weight of 4000-10000 with allyl epoxy polyether with the molecular weight of 500-1000, adding chloroplatinic acid, heating to 100-120 ℃, and reacting for 3-6 hours to obtain double epoxy end-capped polyether silicone oil; (4) And reacting the double epoxy end-capped polyether silicone oil with amine ether with low molecular weight to obtain the low VOC silicone oil. The preparation method does not adopt a solvent, and the fabric treated by the method has full hand feeling, realizes green and environment protection, and reaches the national VOC emission standard.
Description
Technical Field
The invention relates to the technical field of silicone oil, in particular to low-VOC silicone oil and a preparation method thereof.
Background
Amino silicone oil is widely used as a softening agent in various processes of weaving, dyeing and finishing, sewing and the like in textile industry, and is one of the indispensable raw materials for high added value and high functionalization of natural fiber products (such as cotton, hemp, silk, wool fabrics and the like) and synthetic fiber products (such as polyester, polyamide, polyacrylonitrile and the like). The amino silicone oil and the modified amino silicone oil can endow the fabric with special hand feeling, and meanwhile, the problems of oil drift demulsification, roller sticking, yellowing and the like are difficult to avoid in the use process. In recent years, block silicone oils have been increasingly popular in the market, and their excellent low yellowing property and stability make up for the shortages of amino silicone oils, even in terms of hand feel, hydrophilicity and durability. In the process of synthesizing the block silicone oil, D4 (octamethyl cyclotetrasiloxane) and an epoxy end capping agent are generally used as raw materials to synthesize epoxy silicone oil, and then the epoxy silicone oil and polyether amine are used to synthesize ternary copolymer silicone oil. With the national requirements on the VOC (volatile organic compound) in the tail gas discharged by factories, the exceeding emission is forbidden to reduce the pollution to the atmosphere, so that the chemical auxiliary agents used by the factories are required to reach the national VOC emission standard. Therefore, in the aspect of finishing handfeel auxiliary agents, it is necessary to develop a silicone oil with very low emission so as to meet the requirements of national emission standards.
Disclosure of Invention
The invention aims to provide low-VOC silicone oil and a preparation method thereof, wherein the preparation method does not adopt a solvent, and the fabric treated by the low-VOC silicone oil has full hand feeling, realizes green and environment protection, and reaches the national VOC emission standard.
In order to achieve the above object, the present invention provides a method for preparing a low VOC silicone oil, comprising the steps of:
(1) Mixing octamethyltetrasiloxane and hydrogen-containing double seal heads, adding concentrated sulfuric acid, and reacting at 30-45 ℃ to obtain hydrogen-containing silicone oil;
(2) Neutralizing the hydrogen-containing silicone oil at the end by adding sodium carbonate, filtering, and then vacuumizing at high temperature to obtain the hydrogen-containing silicone oil at the end of the low ring body;
(3) Mixing low-ring-end hydrogen-containing silicone oil with the molecular weight of 4000-10000 with allyl epoxy polyether with the molecular weight of 500-1000, adding chloroplatinic acid, heating to 100-120 ℃, and reacting for 3-6 hours to obtain double epoxy end-capped polyether silicone oil;
(4) The double epoxy end capped polyether silicone oil is reacted with amine ether with low molecular weight to prepare the low VOC silicone oil.
In some embodiments, in step (1), the mass ratio of octamethyltetrasiloxane to hydrogen-containing double head is 100:0.5-2. For example, the mass ratio of octamethyltetrasiloxane to hydrogen-containing double heads may be, but is not limited to, 100:0.5, 100:1, 100:1.5, 100:2.
In some embodiments, in step (2), the vacuum is pulled at a temperature of 140-180 ℃ for 1-3 hours, illustratively, but not limited to, 3 hours at 140 ℃, 2 hours at 160 ℃, or 1 hour at 180 ℃. It should be noted that, because the end hydrogen-containing silicone oil also contains a D4 ring, the D4 ring can be removed greatly by adding sodium carbonate for neutralization and filtering and then vacuumizing at 140-180 ℃ for 1-3 hours, so that the ring content is very low, and the high-temperature vacuumizing time is not too long, otherwise, the activity of H at two ends of the product is influenced, the subsequent reaction is not facilitated, the time is too short, and the effect is not ideal.
In some embodiments, the mass ratio of the low ring end hydrogen containing silicone oil to the allyl epoxy polyether is 5-10:1. Illustratively, the mass ratio of the low ring end hydrogen containing silicone oil to the allyl epoxy polyether may be, but is not limited to, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1.
In some embodiments, the allylic epoxy polyether has the following structural formula:
wherein, c is more than or equal to 15 and more than or equal to 5, d is more than or equal to 10 and more than or equal to 6.
Illustratively, the weight average molecular weight of the allyl epoxy polyether can be, but is not limited to, 500, 600, 700, 800, 900, 1000. Further, the allyl epoxy polyether is selected from APEG580, APEG700, APEG800, APEG900, but not limited thereto.
In some embodiments, the amine ether has a weight average molecular weight of 100-1000, illustratively, the amine ether may have a weight average molecular weight of, but not limited to, 100, 200, 300, 400, 500, 600, 700, 800, 900, 1000. Further, the amine ether is at least one selected from tetramethyl propylene diamine, di-dimethylamino ethyl ether, hangzhou QionTt 600, henschel 410, henschel 230, diethylenetriamine and Henschel 400. Exemplary amine ethers are tetramethyl propylene diamine or henlsmeid 400, and the like. It is notable that the amine ether is selected from tertiary amine type, has low alkalinity, can avoid side reaction to cause linear Si-O chain to be closed into a ring, can avoid generating a ring body, and can obtain environment-friendly low-ring product, thereby being beneficial to the subsequent preparation of low-VOC silicone oil.
In some embodiments, in step (4), the mass ratio of the epoxy-terminated polyether silicone oil to the amine ether is 100:5-50, preferably the mass ratio of the epoxy-terminated polyether silicone oil to the amine ether is 100:20-50, and for example, the mass ratio of the epoxy-terminated polyether silicone oil to the amine ether is 100:20, 100:25, 100:30, 100:40, 100:50, and specifically can be practically set according to different molecular weights of the amine ether.
In some embodiments, in step (4), the reaction temperature is 80-95 ℃, as exemplified by, but not limited to 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃, 85 ℃, 86 ℃, 87 ℃, 88 ℃, 89 ℃, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃.
In one embodiment, the amine ether is exemplified by tetramethyl propylenediamine, which illustrates the reaction mechanism of the present invention as follows: step (1):
step (3):
correspondingly, the invention also provides low-VOC silicone oil which is prepared by adopting the preparation method of the low-VOC silicone oil.
The invention has the beneficial effects that:
according to the preparation method of the low-VOC silicone oil, the terminal hydrogen-containing silicone oil is prepared by octamethyltetrasiloxane and a hydrogen-containing double end socket, then the terminal hydrogen-containing silicone oil is neutralized by adding sodium carbonate, filtered, and vacuumized at a high temperature, most of D4 ring bodies can be basically removed under the process, the content of the D4 ring bodies is low to obtain the low-ring-body terminal hydrogen-containing silicone oil, the low-ring-body terminal hydrogen-containing silicone oil with the specific molecular weight of 4000-10000 is mixed with allyl epoxy polyether with the low molecular weight of 500-1000, the reaction is carried out at a higher temperature (100-120 ℃) to obtain the double epoxy end-capped polyether silicone oil, and finally the double epoxy end-capped polyether silicone oil is reacted with amine ether with the low molecular weight to obtain the low-VOC silicone oil.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A preparation method of low VOC silicone oil comprises the following steps:
(1) Sequentially adding 100g of octamethyltetrasiloxane and 1g of hydrogen-containing double seal heads into a reaction bottle, adding concentrated sulfuric acid, and reacting at 40 ℃ for 24 hours to prepare terminal hydrogen-containing silicone oil with molecular weight of 5000;
(2) Adding sodium carbonate into the terminal hydrogen-containing silicone oil for neutralization, filtering, and then vacuumizing at a high temperature of 160 ℃ for 2 hours to obtain low-ring terminal hydrogen-containing silicone oil;
(3) Adding low-ring-end hydrogen-containing silicone oil with molecular weight of 5000 and mass of 60g and allyl epoxy polyether APEG800 with molecular weight of 800 and mass of 10g into a reaction bottle, heating to 100 ℃, preserving heat for 1 hour, adding chloroplatinic acid, and reacting for 5 hours to obtain double epoxy end-capped polyether silicone oil;
(4) 100g of double epoxy end capped polyether silicone oil and 25g of tetramethyl propylene diamine are sequentially added into a reaction bottle to react at the temperature of 85 ℃ for 12 hours, so as to prepare the low VOC silicone oil.
Example 2
A preparation method of low VOC silicone oil comprises the following steps:
(1) Sequentially adding 100g of octamethyltetrasiloxane and 1.2g of hydrogen-containing double seal heads into a reaction bottle, adding concentrated sulfuric acid, and reacting at 30 ℃ for 24 hours to obtain terminal hydrogen-containing silicone oil with a molecular weight of 6000;
(2) Adding sodium carbonate into the terminal hydrogen-containing silicone oil for neutralization, filtering, and then vacuumizing at a high temperature of 160 ℃ for 3 hours to obtain low-ring terminal hydrogen-containing silicone oil;
(3) Adding low-ring-end hydrogen-containing silicone oil with the molecular weight of 6000 and the mass of 90g and allyl epoxy polyether APEG700 with the molecular weight of 700 and the mass of 10g into a reaction bottle, heating to 120 ℃, preserving heat for 1 hour, adding chloroplatinic acid, and reacting for 5 hours to obtain double epoxy end-capped polyether silicone oil;
(4) 100g of double epoxy end capped polyether silicone oil and 20g of Hensmeid 230 are sequentially added into a reaction bottle to react for 12 hours at the temperature of 85 ℃ to prepare the low VOC silicone oil.
Example 3
A preparation method of low VOC silicone oil comprises the following steps:
(1) Sequentially adding 100g of octamethyltetrasiloxane and 1g of hydrogen-containing double seal heads into a reaction bottle, adding concentrated sulfuric acid, and reacting at 40 ℃ for 24 hours to prepare terminal hydrogen-containing silicone oil with molecular weight of 5000;
(2) Adding sodium carbonate into the terminal hydrogen-containing silicone oil for neutralization, filtering, and then vacuumizing at a high temperature of 180 ℃ for 1 hour to obtain low-ring terminal hydrogen-containing silicone oil;
(3) Adding low-ring-end hydrogen-containing silicone oil with molecular weight of 5000 and mass of 50g and allyl epoxy polyether APEG580 with molecular weight of 580 and mass of 10g into a reaction bottle, heating to 100 ℃, preserving heat for 1 hour, adding chloroplatinic acid, and reacting for 5 hours to obtain double epoxy end-capped polyether silicone oil;
(4) 100g of double epoxy end capped polyether silicone oil and 30g of Henschel D400 are sequentially added into a reaction bottle to react at 90 ℃ for 12 hours, so as to prepare the low VOC silicone oil.
Taking the low VOC silicone oil obtained in the examples 1-3, respectively marking the low VOC silicone oil as a sample A1, a sample A2 and a sample A3, respectively weighing the mass of each of the sample A1, the sample A2 and the sample A3, marking the mass as an initial mass m1, respectively putting the sample A1, the sample A2 and the sample A3 into an oven for drying at 180 ℃ for 30 minutes, respectively weighing the mass of each of the sample A1, the sample A2 and the sample A3 after cooling, marking the mass as a final mass m2, and calculating according to the following formula:
α= (m 1-m 2)/m1×100%, and the test results are shown in table 1.
Wherein:
if alpha is less than or equal to 0.5%, the silicone oil is indicated to belong to low VOC silicone oil;
if alpha is more than 0.5%, the silicone oil is not the low VOC silicone oil.
Table 1 test results
From the test results in Table 1, it is clear that the low VOC silicone oils obtained in examples 1-3 of the present invention all have an alpha value of less than 0.5%, are low VOC silicone oils, and meet the national VOC emission standards.
The low VOC silicone oils obtained in examples 1-3 were formulated into a finish B1, a finish B2, a finish B3, the specific compositions and amounts shown in Table 2.
TABLE 2 Components and contents of the finishing agents B1, B2, B3
The cotton fiber fabrics were post-finished with the finishing agents B1, B2 and B3, respectively, and then tested for performance, with reference to table 3, and the blank control was performed with water.
The test items and methods are as follows:
hydrophilicity: by adopting a static drip method, 1 drop of water is dripped from a position 1cm away from the fabric by using a standard dropper (25 drops/mL), and the hydrophilicity is judged by the time for the water drop to be completely absorbed, wherein the shorter the time is, the better the hydrophilicity is.
Feel test: by adopting a physical hand feeling assessment method, a finished cloth sample is cooled and rewet, and is comprehensively assessed by a plurality of qualified hand feeling assessment professionals from the aspects of smoothness, softness, bulk and the like, the hand feeling of the original cloth is set to be 1 minute, the hand feeling assessment is preferably 5 minutes, and the average value is taken.
Stability test: centrifuging the finishing agents B1, B2 and B3 respectively, and storing for 24 hours to check whether layering occurs; the centrifugation conditions were 3000r/min,30min.
TABLE 3 test results
From the test results in table 3, the hand feeling of the blank sample is 1 minute, and the hand feeling of the fabrics treated by the finishing agent B1, the finishing agent B2 and the finishing agent B3 is greatly improved, and the fabrics are full and soft in hand feeling and good in hydrophilicity and stability.
The present invention is not limited to the above embodiments, but is capable of being modified or varied in all embodiments without departing from the spirit and scope of the invention.
Claims (7)
1. The preparation method of the low-VOC silicone oil is characterized by comprising the following steps:
(1) Mixing octamethyltetrasiloxane with hydrogen-containing double seal heads, adding concentrated sulfuric acid, and reacting at 30-45 ℃ to obtain hydrogen-containing silicone oil;
(2) Adding sodium carbonate into the hydrogen-containing silicone oil at the end for neutralization, filtering, and vacuumizing at 140-180 ℃ for 1-3 hours to obtain the hydrogen-containing silicone oil at the end of the low ring body;
(3) Mixing the low-ring-end hydrogen-containing silicone oil with the molecular weight of 4000-10000 with allyl epoxy polyether with the molecular weight of 500-1000, adding chloroplatinic acid, heating to 100-120 ℃, and reacting for 3-6 hours to obtain double epoxy end-capped polyether silicone oil;
(4) Reacting the double epoxy end capped polyether silicone oil with amine ether with low molecular weight, wherein the weight average molecular weight of the amine ether is 100-1000, so as to prepare low VOC silicone oil;
in the step (3), the structural formula of the allyl epoxy polyether is as follows:
wherein, c is more than or equal to 15 and more than or equal to 5, d is more than or equal to 10 and more than or equal to 6.
2. The method for preparing a low VOC silicone oil according to claim 1, wherein in step (1), the mass ratio of the octamethyltetrasiloxane to the hydrogen-containing double cap is 100:0.5-2.
3. The method for preparing a low VOC silicone oil according to claim 1, wherein in step (3), the mass ratio of the low ring end hydrogen-containing silicone oil to the allyl epoxy polyether is 5 to 10:1.
4. The method for preparing a low VOC silicone oil according to claim 1, wherein the amine ether is at least one selected from the group consisting of tetramethyl propane diamine, bis-dimethylamino ethyl ether, huntington QT600, huntington 410, huntington D230, diethylenetriamine, and huntington D400.
5. The method for preparing a low VOC silicone oil according to claim 1, wherein in step (4), the mass ratio of the double epoxy-terminated polyether silicone oil to the amine ether is 100:5-50.
6. The method for preparing a low VOC silicone oil according to claim 1, wherein in step (4), the reaction temperature is 80-95 ℃.
7. A low VOC silicone oil characterized by being produced by the process for producing a low VOC silicone oil according to any one of claims 1 to 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211691596.5A CN115772266B (en) | 2022-12-26 | 2022-12-26 | Low-VOC silicone oil and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211691596.5A CN115772266B (en) | 2022-12-26 | 2022-12-26 | Low-VOC silicone oil and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115772266A CN115772266A (en) | 2023-03-10 |
| CN115772266B true CN115772266B (en) | 2024-02-06 |
Family
ID=85393065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211691596.5A Active CN115772266B (en) | 2022-12-26 | 2022-12-26 | Low-VOC silicone oil and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115772266B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617863A (en) * | 2012-03-30 | 2012-08-01 | 广东工业大学 | Preparation method of hydrophilic block polyether aminosilicone |
| CN104031269A (en) * | 2014-05-20 | 2014-09-10 | 江阴市诺科科技有限公司 | Hydrophilic block polyether amino silicone oil with amino branched chain, and preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111819222B (en) * | 2018-11-20 | 2022-05-31 | 瓦克化学股份公司 | Block modified polysiloxane and composition thereof |
-
2022
- 2022-12-26 CN CN202211691596.5A patent/CN115772266B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617863A (en) * | 2012-03-30 | 2012-08-01 | 广东工业大学 | Preparation method of hydrophilic block polyether aminosilicone |
| CN104031269A (en) * | 2014-05-20 | 2014-09-10 | 江阴市诺科科技有限公司 | Hydrophilic block polyether amino silicone oil with amino branched chain, and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115772266A (en) | 2023-03-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110747649B (en) | Hydrophilic deepening organic silicon softening agent, preparation method and fabric | |
| CN107814941B (en) | Microwave preparation method of smooth quaternary ammonium block organic silicon polymer | |
| CN110820353B (en) | Hydrophilic silicone oil and preparation method thereof | |
| CN114592360B (en) | Polyester fabric solvent dyeing method based on high-molecular printing and dyeing auxiliary | |
| CN110372868B (en) | Preparation method of low-discoloration piperazinyl terminated ester amide polyether modified block silicone oil | |
| CN103333332B (en) | A kind of preparation method of dyeing promoter and application thereof | |
| CN105755834A (en) | Novel washable flame-retardant coating and preparation method thereof | |
| CN106046316B (en) | A kind of preparation method and products thereof of the crosslinked tree-shaped cladodification cationic silicone microemulsion of low-density | |
| CN107522866A (en) | A kind of preparation method of solvent-free block silicone oil | |
| CN115772266B (en) | Low-VOC silicone oil and preparation method thereof | |
| CN113372558A (en) | Preparation method and application process of anion block silicone oil capable of dyeing in one bath | |
| CN102634036A (en) | Novel linear amino and polyester modified organosilicon compound for textiles | |
| CN114855461A (en) | Organic silicon softening agent, preparation method thereof and application thereof in deep color fabric | |
| CN115073743A (en) | Modified organic silicon high polymer material and preparation method thereof | |
| CN107857862A (en) | A kind of preparation method of dication type organic silicon modified aqueous polyurethane color fixing agent | |
| CN106336498B (en) | Hydrolysis resistance agent for fluorine-silicon modified polyurethane artificial leather and preparation method thereof | |
| CN114133573A (en) | Environment-friendly odorless hydrophilic organic silicon softening agent for wool tops and preparation method thereof | |
| CN114106337B (en) | Ternary polymerization hydrophilic amino silicone oil, preparation method thereof and finishing agent | |
| CN106496569B (en) | A kind of permanent hydrophilic silicone oil and preparation method thereof | |
| CN109439056B (en) | Nonionic associative type water-based polyurethane thickener and preparation method thereof | |
| CN115926173B (en) | Low-ring silicone oil and preparation method thereof | |
| CN114182535B (en) | Organic silicon finishing agent with thermal stability | |
| CN112981963B (en) | Net-shaped association type polyurethane composite modified organic silicon softener emulsion and preparation method thereof | |
| CN112680971A (en) | Fabric with excellent performance and application thereof in field of clothes | |
| CN112961355A (en) | Preparation method and application of polyamino vinyl silicone oil |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |