CN115772266A - Low-VOC silicone oil and preparation method thereof - Google Patents
Low-VOC silicone oil and preparation method thereof Download PDFInfo
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- CN115772266A CN115772266A CN202211691596.5A CN202211691596A CN115772266A CN 115772266 A CN115772266 A CN 115772266A CN 202211691596 A CN202211691596 A CN 202211691596A CN 115772266 A CN115772266 A CN 115772266A
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 32
- 239000001257 hydrogen Substances 0.000 claims abstract description 32
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 32
- 229920000570 polyether Polymers 0.000 claims abstract description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000004593 Epoxy Substances 0.000 claims abstract description 17
- 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 14
- 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
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000005086 pumping Methods 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 238000006386 neutralization reaction 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
- 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 16
- 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 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000012855 volatile organic compound Substances 0.000 description 30
- 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 6
- 229920013822 aminosilicone Polymers 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- BPINJMQATUWTID-UHFFFAOYSA-N 3,3-dimethylpentane-2,2-diamine Chemical group CCC(C)(C)C(C)(N)N BPINJMQATUWTID-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 239000000654 additive Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 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
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 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
- 238000011056 performance test Methods 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
- 238000012430 stability testing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 150000003512 tertiary amines Chemical group 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000009489 vacuum treatment Methods 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 low VOC silicone oil and a preparation method thereof, and the preparation method comprises the following steps: (1) Mixing octamethyltetrasiloxane and hydrogen-containing double-end socket, adding concentrated sulfuric acid, and reacting at 30-45 ℃ to prepare hydrogen-containing silicone oil; (2) Adding sodium carbonate into the hydrogen-containing silicone oil at the end for neutralization, filtering, and then carrying out vacuum pumping treatment at high temperature to prepare the hydrogen-containing silicone oil at the end of the low ring body; (3) Mixing the hydrogen-containing silicone oil with the molecular weight of 4000-10000 at the end of the low ring body 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 diepoxy terminated polyether silicone oil; (4) And reacting the diepoxy terminated polyether silicone oil with low molecular weight amine ether to obtain the low VOC silicone oil. The preparation method does not adopt solvents, and the fabrics treated by the method have full hand feeling, thereby realizing green environmental protection and reaching the national VOC emission standard.
Description
Technical Field
The invention relates to the technical field of silicone oil, and particularly relates 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 the textile industry, and is one of essential raw materials for high added value and high functionality of natural fiber products (such as cotton, hemp, silk, wool 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 endow the fabric with special hand feeling, and simultaneously, the problems of floating oil demulsification, roll sticking, yellowing and the like are difficult to avoid in the use process. In recent years, block silicone oils have become popular in the market, and their superior low yellowing property and stability make up for the deficiencies of amino silicone oils, even surpassing amino silicone oils in terms of hand, hydrophilicity and durability. In the synthesis process of the block silicone oil, D4 (octamethylcyclotetrasiloxane) and an epoxy end-capping reagent are generally used as raw materials to synthesize epoxy silicone oil, and then the epoxy silicone oil and polyether amine are used to synthesize the terpolymer silicone oil. With the national requirement on the VOC (volatile organic compound) in the tail gas discharged by the factory, the excessive discharge is forbidden to reduce the pollution to the atmosphere, so that the chemical additives used by the factory are required to reach the national VOC discharge standard. Therefore, in the aspect of finishing the hand feeling auxiliary agent, a silicone oil with low emission needs to be developed 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, the preparation method does not adopt a solvent, and fabrics treated by the low-VOC silicone oil are full in hand feeling, green and environment-friendly effects are realized, and the low-VOC silicone oil 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) Adding sodium carbonate into the hydrogen-terminated silicone oil for neutralization, filtering, and then carrying out vacuum pumping treatment at high temperature to prepare low-ring-body-terminated hydrogen-terminated silicone oil;
(3) Mixing hydrogen-containing silicone oil with the molecular weight of 4000-10000 at the end of a low ring body 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 diepoxy terminated polyether silicone oil;
(4) Reacting the diepoxy terminated polyether silicone oil with low molecular weight amine ether to prepare the low VOC silicone oil.
In some embodiments, in step (1), the mass ratio of octamethyltetrasiloxane to hydrogen-containing double head is from 100. Illustratively, the mass ratio of octamethyltetrasiloxane to hydrogen-containing bis-head can be, but is not limited to, 100.
In some embodiments, step (2) is evacuated at a temperature of 140-180 ℃ for 1-3 hours, illustratively at a temperature of 140 ℃ for 3 hours, at a temperature of 160 ℃ for 2 hours, or at a temperature of 180 ℃ for 1 hour, but not limited thereto. It should be noted that, because the terminal hydrogen-containing silicone oil also contains a D4 ring body, the D4 ring body can be greatly removed by adding sodium carbonate for neutralization, filtering, and then performing vacuum pumping at 140-180 ℃ for 1-3 hours, so that the ring body content is very low, and it is worth noting that the high-temperature vacuum pumping time cannot be too long, otherwise the activity of H at both ends of the product is affected, which is not beneficial to the subsequent reaction, and the effect is not ideal if the time is too short.
In some embodiments, the mass ratio of the low ring end hydrogen-containing silicone oil to the allyl epoxy polyether is 5-10. Illustratively, the mass ratio of the hydrogen-containing silicone oil at the end of the low ring body to the allyl epoxy polyether can be, but is not limited to, 5.
In some embodiments, the allyl epoxy polyether has the following structural formula:
wherein c is more than or equal to 15 and more than or equal to 5, and d is more than or equal to 10 and more than or equal to 6.
Illustratively, the allyl epoxy polyether may have a weight average molecular weight of, but not limited to, 500, 600, 700, 800, 900, 1000. Further, allyl epoxy polyether is selected from, but not limited to, APEG580, APEG700, APEG800, APEG 900.
In some embodiments, the amine ether has a weight average molecular weight of 100 to 1000, illustratively, the amine ether can have a weight average molecular weight of, but is not limited to, 100, 200, 300, 400, 500, 600, 700, 800, 900, 1000. Further, the amine ether is at least one selected from tetramethylpropylenediamine, bisdimethylaminoethylether, hangzhou Qiongtian QT600, hunsmei ED410, hunsmei D230, diethylenetriamine and Hunsmei D400. Illustratively, the amine ether is tetramethylpropanediamine or hensimei D400, or the like. The amine ether is selected from tertiary amine type, the alkalinity is low, side reaction can be avoided, linear Si-O chain is closed to form a ring, ring body generation can be avoided, an environment-friendly low-ring product is obtained, and the preparation of the follow-up low-VOC silicone oil is facilitated.
In some embodiments, in step (4), the mass ratio of the diepoxy terminated polyether silicone oil to the amine ether is from 100 to 50, preferably the mass ratio of the diepoxy terminated polyether silicone oil to the amine ether is from 100 to 50, and the mass ratio of the diepoxy terminated polyether silicone oil to the amine ether is from 100 to 20, 100, 30, 100, 40, 100.
In some embodiments, the reaction temperature in step (4) is 80-95 ℃, and illustratively, the temperature may be, but is 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 tetramethylpropanediamine as an example to illustrate the reaction mechanism of the present invention, as follows: step (1):
and (3):
correspondingly, the invention also provides low-VOC silicone oil prepared by the preparation method of the low-VOC silicone oil.
The invention has the following beneficial effects:
according to the preparation method of the low VOC silicone oil, the hydrogen-terminated silicone oil is prepared through octamethyltetrasiloxane and a hydrogen-containing double end enclosure, then the hydrogen-terminated silicone oil is neutralized by adding sodium carbonate, the filtration is carried out, then the vacuum treatment is carried out at high temperature, most of D4 ring bodies can be basically removed under the process, the content of the D4 ring bodies is low, the low ring body end hydrogen-containing silicone oil is obtained, then the low ring body end hydrogen-containing silicone oil with specific molecular weight of 4000-10000 and the allyl epoxy polyether with low molecular weight of 500-1000 are mixed, the reaction is carried out at higher temperature (100-120 ℃) to obtain the diepoxy end-capped polyether silicone oil, and finally the reaction is carried out with the amine ether with low molecular weight to obtain the low VOC silicone oil.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present 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 hydrogen-containing terminal silicone oil with molecular weight of 5000;
(2) Adding sodium carbonate into hydrogen-terminated silicone oil for neutralization, filtering, and then carrying out vacuum-pumping treatment at the high temperature of 160 ℃ for 2 hours to obtain low-ring-body-terminated hydrogen-terminated silicone oil;
(3) Adding low-ring-end hydrogen-containing silicone oil with the molecular weight of 5000 and the mass of 60g and allyl epoxy polyether APEG800 with the molecular weight of 800 and the mass of 10g into a reaction bottle, heating to 100 ℃, preserving the temperature for 1 hour, adding chloroplatinic acid, and reacting for 5 hours to obtain diepoxy terminated polyether silicone oil;
(4) And sequentially adding 100g of diepoxy terminated polyether silicone oil and 25g of tetramethyl propylene diamine into a reaction bottle to react at the temperature of 85 ℃ for 12 hours to obtain 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 prepare hydrogen-containing terminated silicone oil with the molecular weight of 6000;
(2) Adding sodium carbonate into hydrogen-terminated silicone oil for neutralization, filtering, and then carrying out vacuum-pumping treatment at the high temperature of 160 ℃ for 3 hours to obtain low-ring-body-terminated hydrogen-terminated 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 the temperature for 1 hour, adding chloroplatinic acid, and reacting for 5 hours to obtain diepoxy terminated polyether silicone oil;
(4) And (3) adding 100g of diepoxy terminated polyether silicone oil and 20g of Hensmei D230 into a reaction bottle in sequence, reacting at 85 ℃ for 12 hours to obtain 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 hydrogen-containing terminal silicone oil with molecular weight of 5000;
(2) Adding sodium carbonate into hydrogen-terminated silicone oil for neutralization, filtering, and then carrying out vacuum-pumping treatment at the high temperature of 180 ℃ for 1 hour to obtain low-ring-body-terminated hydrogen-terminated silicone oil;
(3) Adding low-ring-end hydrogen-containing silicone oil with the molecular weight of 5000 and the mass of 50g and allyl epoxy polyether APEG580 with the molecular weight of 580 and the mass of 10g into a reaction bottle, heating to 100 ℃, preserving the temperature for 1 hour, adding chloroplatinic acid, and reacting for 5 hours to obtain diepoxy terminated polyether silicone oil;
(4) And sequentially adding 100g of diepoxy terminated polyether silicone oil and 30g of Hounsfield D400 into a reaction bottle for reaction at the temperature of 90 ℃ for 12 hours to obtain the low-VOC silicone oil.
Taking the low-VOC silicone oil obtained in the examples 1 to 3 and respectively marking as a sample A1, a sample A2 and a sample A3, respectively weighing the respective masses of the sample A1, the sample A2 and the sample A3 and marking as an initial mass m1, then respectively putting the sample A1, the sample A2 and the sample A3 into an oven to be dried at 180 ℃ for 30 minutes, respectively weighing the respective masses of the sample A1, the sample A2 and the sample A3 after cooling, marking as a final mass m2, and calculating according to the following formula:
α = (m 1-m 2)/m 1 × 100%, and the test results are shown in table 1.
Wherein:
if alpha is less than or equal to 0.5 percent, the silicone oil is low VOC silicone oil;
if alpha is more than 0.5 percent, the silicone oil is not low VOC silicone oil.
TABLE 1 test results
From the test results in table 1, it can be seen that the α values of the low VOC silicone oils obtained in examples 1 to 3 of the present invention are all less than 0.5%, and the low VOC silicone oils belong to low VOC silicone oils and meet the national VOC emission standards.
The low-VOC silicone oils obtained in examples 1 to 3 were formulated into finish B1, finish B2 and finish B3, the specific components and contents of which are shown in Table 2.
TABLE 2 Components and contents of finish B1, B2, B3
Finishing agent B1, finishing agent B2 and finishing agent B3 are respectively taken to carry out after-finishing on the cotton fiber fabric, then performance test is carried out, the result refers to table 3, and blank control is carried out by adopting water.
The test items and methods were as follows:
hydrophilicity: the hydrophilicity was judged by dropping 1 drop of water from a position 1cm from the fabric using a standard dropper (25 drops/mL) by the static drip method, and the shorter the time, the better the hydrophilicity was.
Hand feeling test property: and (3) a physical hand feeling evaluation method is adopted, the finished cloth sample is cooled and remoistened, and the original cloth hand feeling is rated as 1 point through comprehensive evaluation of multiple qualified hand feeling evaluation professionals from the aspects of smoothness, softness, filling power and the like, the hand feeling evaluation is preferably rated as 5 points, and the average value is taken.
And (3) stability testing: after the finishing agents B1, B2 and B3 are respectively centrifuged and stored for 24 hours, whether the layering phenomenon occurs or not is checked; the centrifugation condition is 3000r/min,30min.
TABLE 3 test results
From the test results in table 3, the hand feeling of the blank sample is 1 point, and the hand feeling of the fabric treated by the finishing agent B1, the finishing agent B2 and the finishing agent B3 is greatly improved, and the fabric is full and soft in hand feeling, and good in hydrophilicity and stability.
Although the present invention has been described with reference to the preferred embodiments, 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 preparation method of the low VOC silicone oil is characterized by comprising the following steps:
(1) Mixing octamethyltetrasiloxane and hydrogen-containing double seal heads, adding concentrated sulfuric acid, and reacting at 30-45 ℃ to prepare hydrogen-containing silicone oil;
(2) Adding sodium carbonate into the hydrogen-containing silicone oil at the end for neutralization, filtering, and then carrying out vacuum pumping treatment at high temperature to prepare the hydrogen-containing silicone oil at the end of the low ring body;
(3) Mixing the hydrogen-containing silicone oil with the molecular weight of 4000-10000 at the end of the low ring body 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 diepoxy terminated polyether silicone oil;
(4) And reacting the diepoxy terminated polyether silicone oil with low molecular weight amine ether to obtain the low VOC silicone oil.
2. The method for preparing the low VOC silicone oil of claim 1, wherein in the step (1), the mass ratio of the octamethyltetrasiloxane to the hydrogen-containing double end enclosure is 100.5-2.
3. The method for preparing the low VOC silicone oil of claim 1, wherein in the step (2), the vacuum is applied at a temperature of 140 to 180 ℃ for 1 to 3 hours.
4. The method for preparing a low VOC silicone oil according to claim 1, wherein in step (3), the mass ratio of the low cyclic end hydrogen-containing silicone oil to the allyl epoxy polyether is 5-10.
5. The method for preparing the low VOC silicone oil according to claim 1, wherein in step (3), the allyl epoxy polyether has the following structural formula:
wherein c is more than or equal to 15 and more than or equal to 5, and d is more than or equal to 10 and more than or equal to 6.
6. The method for producing a low VOC silicone oil as claimed in claim 1, wherein in step (4), said amine ether has a weight average molecular weight of 100 to 1000.
7. The method according to claim 6, wherein the amine ether is at least one selected from the group consisting of tetramethylpropylenediamine, bisdimethylaminoylethyl ether, hangzhou Qiongtian QT600, hunsmei ED410, hunsmei D230, diethylenetriamine and Hunsmei D400.
8. The method for preparing the low VOC silicone oil of claim 1, wherein in the step (4), the mass ratio of the diepoxy terminated polyether silicone oil to the amine ether is 100.
9. The method for preparing the low VOC silicone oil of claim 1, wherein in the step (4), the reaction temperature is 80 to 95 ℃.
10. A low VOC silicone oil characterized by being produced by the method for producing a low VOC silicone oil according to any one of claims 1 to 9.
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Citations (3)
| 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 |
| US20210388163A1 (en) * | 2018-11-20 | 2021-12-16 | Wacker Chemie Ag | Block-modified polysiloxanes and compositions formed thereof |
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- 2022-12-26 CN CN202211691596.5A patent/CN115772266B/en active Active
Patent Citations (3)
| 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 |
| US20210388163A1 (en) * | 2018-11-20 | 2021-12-16 | Wacker Chemie Ag | Block-modified polysiloxanes and compositions formed thereof |
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